HOME CHEMISTRY THREAD

[OP !t9hZgTuuXA No.3328052]

Home chemistry thread! /sci/entists get in here, let's discuss home chemistry/home labs.

Pic related, it's an ongoing nitrobenzene synthesis.

[Anonymous No.3328072]

>pour hydrogen peroxide onto cut
>watch it react with catalase enzyme
>SCIENCE

[Anonymous No.3328076]

HOW DOES I MAKE METH?

[OP !t9hZgTuuXA No.3328087]

>>3328072

Come over to my place and we'll do some science.

[Anonymous No.3328105]

OP where do you get your glassware and chemicals, regardless of what your synthesizing doesn't it draw unwanted attention?

[Anonymous No.3328108]

>>3328087
damn nigga u got that good shit.

[OP !t9hZgTuuXA No.3328128]

>>3328105

If you live in the US I can understand your concern, with the war on drugs and all that shit. The rest of the world is more relaxed in that regard. In Norway I have no problems getting chemicals and glassware from large suppliers, but if you were to do that in the US chances are that you'd be reported to the DEA.

eBay is a good place to start. Used quality glassware is cheap, as well as basic (especially inorganic) reagents. expediglass.com, unitedglasstech.com both sell cheap jointed glassware.

[OP !t9hZgTuuXA No.3328140]

>>3328105
Also, with regards to "unwanted attention" - I already have attention. :) To buy chemicals labeled "toxic" or "very toxic" I need a to hand in a police permit to the supplier (which I have done three times), so I'm already in their databases.

[Anonymous No.3328155]

>>3328076
Watch the entire 1st season of Breaking Bad and you should be good to go

[Anonymous No.3328159]

>>3328140
>>3328128
OP sounds like he knows what hes talking about, and yes i live in the US and you pretty much explained the situation here. what chemicals do you have to get a license for? and what do you use for a reducing agent on your synthesis

[Anonymous No.3328204]

>>3328072
No the bubbling means there was bacteria in the woundz and it was infected!!!!!!

/end stupid shit I hear all the time

[OP !t9hZgTuuXA No.3328287]

>>3328159

Methanol, dichloromethane and white phosphorus (!). I probably have ~10 more chemicals classified as toxic or very toxic, but I got them from my chemistry teacher, thus eliminating the need for any permits... Among them are some rare jewels like HgCl2, CS2, CCl4, some nickel salts and lead acetate. Also, I have some bromine and some benzene, but I made both myself.

Reducing agent? Nitration of benzene is an electrophilic aromatic substitution reaction; there's no reducing agent here. Just benzene, sulfuric acid and nitric acid.

If you meant reducing agents in general, I don't have that many. Tin, zinc and iron powder are useful in some organic reductions as well as tin(II) chloride. Some sodium thiosulfate and sulfite are on my shopping list.

[Anonymous No.3328333]

>>3328287
damn, that is a bit more then i know. i am planning on going to school for chem this fall, i know some stuff, almost all of it is stuff Ive tried to teach my self online, you would happen to have aim or Skype or something? I'm always interested in trying to learn, if you feel like explaining

[Anonymous No.3328344]

>>3328287
btw i assumed you were going to reduce the nitro group to an amine, that's why i asked

[Anonymous No.3328362]

OP, why aren't you busy, synthesizing LSD-25, mescaline or DMT already??

[Hououin Kyouma No.3328377]

Don't buy all your supplies at once. That'll draw too much attention.

[Anonymous No.3328380]

>>3328287
I'm surprised that methanol is something you'd need a permit for. Even in the US, you can just buy it on amazon. Glassware, as well (that's where I got mine).

[Anonymous No.3328388]

>>3328362
>>3328362
>>3328362
>>3328362
fucking this

[OP !t9hZgTuuXA No.3328397]

>>3328333
Skype: chemforsci
Everyone who wants to discuss chemistry is welcome to add me.

>>3328344
That makes more sense. I haven't decided yet, I might use steel wool. But I also have some SnCl2 lying around.

>>3328362
Because I'm not interested in psychedelics, plus the fact that they're not easy to synthesize at all. Amphetamines are easy to make, but it's not something for me.

>>3328380
EU regulations bans methanol for sale to consumers. That and Norwegian law states that you need a special permit to buy anything toxic/very toxic.

[Anonymous No.3328408]

>>3328362


because you cant really synthesize LSD.

it is a "semisynthesis" from an already well constructed natural product.

Ergotamine, ergocristine, etc. are used as precursors. Even if you wanted to do a "home synthesis" and simply use morning glory extract (which would require a fuck-ton of HBW seeds), you would still make a precipitously small amount.

As I have said in other threads where random posters have looked up "LSD synthesis" on google, and found the usual bullshit:

1) create home culture of Ergot (including elaborate descriptions of how to set up sterile conditions, like sucking air through bleach bubblers and stuff)

2) extract ergot alkaloid from ergot (lol, by HAND hahahaha)

3) chop to the carboxylic acid (variety of methods, all will actually destroy or epimerize the ergot into non-reactive materials that stay with the process and are present in the end product)

4) using 1950s chemistry, activate the carboxylic acid (the usual preps list DCC activation, which was used in the 1960s with the first solid phase peptide synthesis schemes)

5) couple with diethylamine


without black-market sourced precursors, you would be risking a particularly dangerous synthesis for a very limited product.

[Anonymous No.3328410]

>>3328397
>Because I'm not interested in psychedelics...

What a pity, would be swell if there was a producer of that sort of stuff here in scandinavia.

[Anonymous No.3328421]

>>3328408

[Anonymous No.3328430]

>>3328344
NEEDS MORE NITRO.

[Anonymous No.3328465]

>>3328076
Theres a couple different ways. All of them are risky, its a volatile chemical and if its made wrong its fumes can really hurt you, not to mention the chance (however small) that it blows up in your chemistry set. The first thing to do is get a house no one will miss and that no one currently lives in, preferably one you can go into without having to ask anyone.

[Anonymous No.3328466]

OP:

synthesize Fentanyl. I have worked out a synthesis that requires the absolute minimum of "difficult or hard to get" chemicals.

you need (difficult/hard to get)

1) 30% H202 (which you already have)
2) Borohydride reducing agent (1-2 mols of it)
3) any one of a long list of oxidizing agents (that will NOT oxidize a primary alcohol to carboxylic acid.)
this is probably the most difficult because not only is it a "drug" type precursor material, but the majority of these things are toxic and bad for the environment (chromium reagents)...

4) propionic acid or propionic acid chloride/anhydride and/or an activating agent + propene (propylene)

5) a Borane reagent (you will perform a hydroboration-oxidation, which is where #1 comes in)
Why do this synthesis?


1) easiest full synthesis (total synthesis) of, realistically any drug you could possibly make

2) about as potent, by weight, as LSD.... so a gram is like the equivalent of 50-100 grams of morphine

make a kilogram and you have many hundreds of thousands of dollars worth of drug material, even if you basically "gave it away" at some hilariously low price

3) The people buying the drug are addicted to it, so you have guaranteed customers.

[Anonymous No.3328498]

>>3328397
DMT is easy, just requires time if you want a good yield.
-http://www.erowid.org/chemicals/dmt/extraction_guide1/dmt_extraction_guide1.shtml
-http://wiki.dmt-nexus.com/Marsofold%27s_tek
-http://www.totse.info/cms/quick-dmt-technique

[Anonymous No.3328516]

>>3328408
http://www.lycaeum.org/leda/docs/8774.shtml?ID=8774
This website has a few methods, haven't tried any but, might work.
LSD-25 btw

[Anonymous No.3328529]

anybody knows how to synthesis mescaline?
i've heard its not that hard

[Anonymous No.3328536]

>>3328529
First link on google :/
http://www.mescaline.com/synth/index.htm

[Anonymous No.3328539]

>>3328516


Once again, as I pointed out in my earlier post, absolutely everything that circulates on the web follows from a similar (or possibly the same) premise:

create your own ergot culture or extract the ergot alkaloids from HBW.

the problems with the first line are:

1) ergot is virulently poisonous

2) ergot does not produce a signficant amount of ergotamine or other ergot alkaloid, so even with a pretty substantial culture, you are not going to produce a very large amount of the starting material

3) maintaining and handling an "industrial sized" ergot culture like this is something that Ph.D. microbiologists struggle to do


the 2nd possibility has some difficulties as well:

1) HBW also has a very small amount of the required ergot alkaloids (you would need many 10s of kilograms to produce sufficient quantities to make any appreciable amount of LSD)

2) it is very difficult to purify the resulting extract without destroying the ergot alkaloids.

[Anonymous No.3328570]

>Went to a lab my father works in as an overseer of sorts
>I was about 19, chem students in college
>see someone in a full suit with two pairs of gloves working in a fume hoods with another pair of laminated gloves
>"Whatcha working with there, an atom bomb?"
>"Dimethylmercury kid."
>Leave and never return

I didn't even ask why they had it, I just didn't want the damn stuff near me.

[OP !t9hZgTuuXA No.3328569]

>>3328498
There's a difference between "extraction" and "total synthesis". I am aware of how acid-base extractions work.

>>3328466
Synthesizing a shit drug and profiting from people's addiction to it is not something I'm willing to do.

Also, I'd like to se a reference to your "synthesis". I can get the reagents needed without any problems.

>>3328408
>>3328539
This guy has done his homework.

[Anonymous No.3328583]

>>3328570
Some strong ass neurotoxin, good thing you didn't breath it in.

[Anonymous No.3328590]

question, in an acid-base extraction, i need to use hcl to acidify the solution. in a later synthesis of hydrobromic acid, i need to use concentrated sulfuric acid.

in the first acid-base extraction, am i able to substitute the hcl with sulfuric acid? does any strong acid do, or does the hcl provide a specific chemical action that sulfuric acid won't?

[None !/oddSpacew No.3328609]

>>3328570
>dat image name
also, I'm pretty sure it's used for calibration.

[Anonymous No.3328610]

OP, why don't you synthesize some MDMA? It's like this:
http://taimapedia.org/index.php?title=A_Complete_MDMA_Synthesis_for_the_First_Time_Chemist

Of course, this is a complete hillbilly method, but with use of prime conditions and chemicals, it could turn out very well.

Sorry for the first deleted post, I used the wrong link.

[Anonymous No.3328619]

>>3328583
>>3328609
Sorry about that you guys, I put that in the wrong thread. But yeah, it's some crazy shit.

And yes, I use long file names.

[Anonymous No.3328622]

come here let me teach you.

first of all you need to get the pseudo (ephedrine), get it in pharmacies or whatever, then we'll need some red phosphorus, could be taken from match boxes, then some iodine.

get all the gear in different places, play low profile, stay off the DEA's highlight.

or we could use reductive amination of phenylacetone but that would require methylamine and stealing a barrell of it wouldn't be a good idea, the feds would be all over you, unless you have a naive brother-in-law whom you can easily deceive

[OP !t9hZgTuuXA No.3328630]

>>3328590
I'm guessing you're forming the hydrochloride salt of an amine. Whether or not you can use sulfuric acid instead of hydrochloric acid depends on the properties of the sulfate salt of the amine.

>>3328610
Because I don't want to break the law. If the police one day decides to show up at my lab, I want to show them a well-organized, clean, safe and legal lab and tell them it's my hobby.

[Anonymous No.3328641]

>>3328610
>Paraformaldehyde
>Using something called Mildewcyde

[Anonymous No.3328643]

>>3328622

Don't I know you from somewhere...

[Anonymous No.3328647]

>>3328630
Where is your lab, if I may ask? As in, do you have a dedicated space for it or make due with what you have?

[Anonymous No.3328663]

>>3328630

actually, i'm trying to form the hcl salt of a tartrate

[Anonymous No.3328664]

>>3328643
no. we've never met before. you've never seen me. carry on.

[OP !t9hZgTuuXA No.3328732]

>>3328647
Heh. It's in my mom's basement. What a stereotype I am. (inb4 neckbeard, 1 inch penis, no girlfriend etc.)

>>3328663
Well that doesn't make sense. Adding a strong acid to a tartrate salt will liberate the free acid. Using H2SO4 instead of HCl shouldn't be a problem, but you have to consider the effects of the anion.

Also, contact me on skype if you want to talk about chemistry: chemforsci
(I won't teach you how to make meth)

[Anonymous No.3328760]

>>3328732

sorry, i was mistaken. the hcl is used in the last step to convert the basic amine to the hcl salt.

i pretty much just answered my own question, didn't i?

[Anonymous No.3328770]

>>3328732

[Anonymous No.3328780]

>>3328569


FYI I (they guy who said make Fentanyl) am the same person you said "did their homework" with respect to the LSD synthesis.

let me point out a few things, before I being the long and arduous post of the specific Fent. synthesis I have dreamed up

1) fentanyl is not a "shit" drug. it is a ridiculously potent synthetic opioid and it is one of the best examples of the modern triumphs of functional design of pharmaceuticals. Fentanyl has its own chapter in pharmaceutical textbooks and it is used as a "historical example" or "historical model" of functional design of pharmaceutically active compounds.


2) my reference to the addiction was more of a joke, and your response indicates you have very limited knowledge of the overall subject and the specifics at hand

if someone synthesizes 1 kilogram of fentanyl... they are not going to be directly "dealing with" addicts. they will be dealing with hardened organized crime members and major drug dealers at the highest or 2nd highest levels of the "drug distribution" pyramid (as opposed to the production/manufacturing part of the industry).

1 kilogram of fentanyl is about the equivalent of ~75 kilograms of pure morphine (or heroin), which means that it is equivalent to about $1,000,000 of heroin or morphine at bulk pricing.
the next post will contain the synthesis procedure. Note: if you have not yet completed (AT LEAST) your 2nd quarter of college level organic chemistry, you will not understand the process without referencing the steps by google searches or textbook inquiry.

it is not conceptually difficult, but it is the stuff covered in the 2nd and 3rd quarter (or 2nd semester) of the traditionally "2nd year" of a chemists undergraduate education.

[Anonymous No.3328788]

>>3328287
Where do you get your nitric acid? I've been making mine myself from fertilizer and sulfuric acid.

[Anonymous No.3328812]

>>3328780


the goal of this synthesis is to avoid the necessity of buying large quantities of extremely "obvious" watched chemicals that are known to be used in the synthesis of fentanyl or other compounds.


A little background:

Fentanyl is a phenylethylamine, just like MDMA, Mescaline, Methamphetamine/amphetamine, DOB, etc.

the phenylethylamine functional group no longer dominates the structural activity of the molecule like it does in the comparatively simple class of phenylethylamines most well known for their roles as recreation drugs, popularized by Shulkin's Pihkal. it is still very relevant to the drugs overall strength and effect, as is evident by the adjustment of this groups structure in the Bentley series. Fluorination, substitution of a benzylic group with a thiophenylic group, etc. have been used to alter the drug's binding efficacy and metabolism rate.

the 2nd bit of background is this: Fentanyl is a well known drug of abuse. It is very well known in all western countries where there are well defined subcultures of opiod drug abusers... With this being the case, any "direct" precursors are heavily watched. They are just about as "watched" as acetic anhydride, safrole oil, ergotamine (or other ergot alkaloids), etc.


Thus, it is advantageous to design a synthesis that avoids direct precursors that are specifically listed as obvious precursors to the compound in question. The disadvantage with this type of procedure is that the "direct" precursors are usually chosen because they achieve the synthesis quickly, easily, and in high yield with low cost.

Thus, some balance must be found between precursors that are not watched, and synthesis that are easy enough to achieve without significant planning and preparative work.

Further consideration must be made for purification and any required "preliminary" steps such as protection/protection of intermediates.

[Anonymous No.3328841]

>>3328812

A little note on purification:


Purification of large quantities of organic chemicals can be extremely difficult. Indeed, one of the things they DO NOT teach you when you are an undergraduate is that in REAL LIFE:

1) You almost NEVER use chromatography to purify large quantities of a reaction mixture.

2) whenever possible, reactions are carried out without solvent or with an absolute bare minimum of solvent

3) if it is necessary to chemically alter a product in order to make purification easy or possible, it is done so almost 100% of the time.

for example: if you can protect an alcohol as a benzylic ether in order to make it precipitate from a solution of reagents and side products, it will be done.

I just wanted to come back to 1:

chromatography is unbearably expensive. Purification of 1 kilogram of a reaction mixture typically requires on the order of 50-100 kilograms of silica/alumina. and many 10s, possibly hundreds of gallons of solvent.

These commercial "flash" columns were usually 1-2 feet in diameter and 20-30 feet tall.

even modern high performance purification methods... such as various high pressure chromatography and tricky "moving bed" chromatography systems are still avoided wherever possible.

Admittedly, within the past 10-15 years, extremely powerful advancements have been made in the field of industrial scale purification methodologies. But these are totally inaccessible to all but the most highly funded multi-national organized crime syndicates.

Unless you have a spare $5,000,000 laying around, and some "legitimate" business front, these types of methods are completely out of the question.

[Anonymous No.3328850]

so with my background setup:

1) no direct precursors if possible

2) cheap reagents (exceedingly cheap)

3) simple reactions

4) simple purifications or the ability to "condense" the number of purifications into a minimum number of steps.


reality time:

1) propionic acid, acid chloride, anhydride, etc. are all watched precursors that are known specifically for their use in the manufacture of fentanyl, and basically nothing else.

2) all of the "associated" reagents, especially the reducing agents are also "watched" chemicals as they are relevant to the synthesis of all of the designer party drugs and methamphetamine.

3) along with the bare minimum, you will need quite a bit of glassware and solvents.

you will also need access to vacuum and inert gas systems.

4) a rotary evaporator would not hurt

[OP !t9hZgTuuXA No.3328858]

>>3328780
I did not mean to "insult" fentanyl like that. It is indeed a triumph of modern organic chemistry and pharmacology, and its clinical potential is incredible. My *personal* view is that fentanyl, like heroin and morphine, are shitty *recreational* drugs. But that may just be my personal taste.

I'm totally blank when it comes to pharmacology/pharmacokinetics. I specialize in organic synthesis.

No matter what you say, I won't synthesize anything illegal and sell it for money.

>>3328788
Chemical suppliers. Sulfuric acid + a nitrate salt is a good route to HNO3.

[Anonymous No.3328901]

>>3328850


reagents needed:

Styrene
parformaldehyde (a polymer of formaldehyde, this is how you purchase formaldehyde... you put it in a flask with a septum, an inert gas inlet, and a cannula to the reaction flask, and heat it causing formaldehyde gas to be evolved and transferred into the reaction flask)
ammonia gas (preferrably) or some other way to generate pure, dry ammonia gas.
acetone (needs to be distilled to dryness and purity, or passed over molecular sieves as in a solvent system)
Aniline (needs to be purified, so distillation from Li or Na wire, as well as storage over a drying agent)
borane reagent. Any will do. Selective reagents like sec-butyl borane or L-selectride are not necessary...
extra dioxane or THF (solvents)
Various common solvents: pet ether/hexanes, dichloromethane, ethyl acetate, acetone, methanol or ethanol, etc.
KOH and HCl would be useful as well.
Drying agent (preferably molecular sieves)
inert gas (preferably argon)


Glassware/tools needed:

flasks of varying sizes... anywhere from 5-10 liter 3-neck reactors to 100 mL round bottoms
stir bars
stir plates
hot plates/oil bath+heater+controller
vacuum source
various syringes and needles; cannulas as well (long double ended needles)
Reflux condensers capable of fitting most of the mid-large flasks, and/or reducing adapters.
if you want to get crazy you could get oxygen-sensitive addition funnel (Looks like OP has one already)
thermometers with adapters for inert handling.

Possibilities:
large separatory funnel and/or a large scale distillation apparatus (vacuum/inert handling: vacuum neck, vacuum condenser, vacuum spout, etc.)
rotary evaporator
largest-possible diameter flash column (probably around 6" to 12" in diameter, commonly called "horse cock" columns due to their immense size).

also TLC plates for reaction monitoring and possibly 1-2 PTLC plates for final chromatographic purification.

[Anonymous No.3328909]

>>3328780

fentanyl is sold as heroin and often uninformed users will not know to adjust their intake and it leads to more overdoses. it is also quite harder to kick than heroin.

[Anonymous No.3328966]

>>3328901

first step is synthesis of acetone dicarboxylic acid.

this is prepared by decarboxylation/oxidation (actually, various sources report it as a decarbonylation, removal of CO rather than CO2) of CITRIC ACID by sulfuric acid under reduced temperatures ~0-10 C.

it is a relatively simple, easy to perform reaction. Just fuming H2SO4, citric acid, and lots and lots of ice... no inert conditions, no ultra dry conditions etc.

Ref:
http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?prep=cv1p0010

2nd step:

this is a variation on the Petrenko-Kritschenko piperidone synthesis

usually you need an inductively stabilized aldehyde like benzaldehyde to achieve this reaction in high yield. But yield is not as important here because the reagents are so cheap.

unfortunately, I do not believe there exists an "oxalic acid mono-aldehyde" that would incorporate the aldehyde functionality with a carboxylic acid that might be labile via decarboxylation, but I digress.


2x aldehyde + >1x ammonia + 1x acetonedicarboxylic acid... room temp, and probably an alcoholic solvent.

personally, I would go with isopropanol or tert-butanol to prevent side reactions with the solvent.

I would expect yields no higher than 10%, but given the extremely low cost nature of the starting materials, I think it is acceptable.

Ref: http://en.wikipedia.org/wiki/Petrenko-Kritschenko_piperidone_synthesis

[Anonymous No.3328972]

>>3328909


that is actually very very old information relevant to the mid 1970s and 1980s when "china white" was relatively new.

this has not been the case for a very long time.

people who DO die from fentanyl overdoses are almost exclusively abusing prescription fentanyl.

[Anonymous No.3329056]

>>3328966


3rd step:

producing 1-phenylethanal (phenyl acetaldehyde)

3a) hydroboration/oxidation of styrene.

Highest theoretical yield is around 80% when you use simple Borane. if you use a selective (sterically hindered) borane reagent like 9-BBN or disamylborane, the theoretical yield jumps to ~98%

again, not a big deal since the reagents are so cheap (styrene, lol DIRT CHEAP).

anyway this is a straight up hydroboration oxidation.end products will be mixed:

1-phenylethanol and 2-phenylethanol.

do not purify, but simply isolate from the aqueous reagents (the boronate, the excess KOH, the excess H2O2, etc.


3b) starting with the mixed product from the previous reaction sequence, we oxidize the phenylethanol(s) to 1-phenylacetaldehyde.

the 1-phenylethanol will be oxidized to acetophenone (methyl-phenyl-ketone)
the 2-phenylethanol will be oxidized to the desired 1-phenylacetaldehyde (phenylacetaldehyde).


alternatively, you could do a Swern/Moffatt and get sole primary alcohol oxidation, "leaving behind" the impurity side product from the previous reaction. Swerns are nice and mild, but they are time consuming and involve more reagents than are necessary.

more realistic "day-to-day" cheap reagents used in "early steps" of multi step synthetic procedures are the Chromium based reagents:

Collins Ratcliff (CrO3-2pyridine in CH2Cl2)
PCC (Pyridinium Chloro Chromate)
PDC (pyridinium dichromate, soluble in H-bonding polar solvents like DMSO/H2O, etc.... Note in DMF it oxidizes all the way to the acid)
DMP oxidation (much more expensive and difficult to get the reagents, also explosive intermediates)
TPAP + N-methyl-morpholineoxide(contains ruthenium, so pretty expensive, but it is also a catalyst, so you only need ~5 mol%)
TEMPO+hypochloride+NaBr+H2O in CH2Cl2

that last one is the best. it is also the most environmentally friendly, safest, etc.

[Anonymous No.3329063]

>>3329056


after oxidation of the mixture of phenylethanols we have:

1-phenylacetaldehyde and acetophenone.


again, we leave them together, and do not isolate them (which is unnecessary and will decrease yield).

we simply isolate them from any regents needed for their oxidation.

this is accomplished (in most cases) by acid base (aqueous/organic) extraction, precipitation, and/or distillation.

[SomeStupidFag !!jgMdkqLZWtJ No.3329368]

>>3329063

Please continue, I'm interested in your procedure.

[Anonymous No.3329537]

>>3329063


step 4:

formation of eneamine as the product of reaction of the 4-piperidone with the phenylacetaldehyde.

the "impurity" acetophenone will, under the appropriate choice of reaction conditions ("kinetic control" meaning lower temperature and shorter reaction time) not undergo significant reaction with.

the desired product is the styryl eneamine

the only possible side product is an extremely unfavorable di-substituted primary alkene eneamine, and this thing basically does not form at all unless you cook the shit out of the reaction mixture.


in this case we would add the amine slowly to a solution of the aldehyde, stirred over molecular sieves, and for good measure under argon.

heating may be necessary to speed the reaction, though refluxing is not needed. best choice is a non-coordinating non-stabilizing solvent.

[Anonymous No.3329550]

>>3329368


sorry dude, got distracted.


anyway, product of previous reaction is the styryl eneamine.
next reaction involves the same exact process, but with the aniline as the amine.


the product of this reaction is a conjugated imine (reacts with the carbonyl group of the 4-pipirodone ring).


same reaction conditions.


indeed, it may be advantageous to simply do this as a "sequential one-pot" reaction.

1st reaction was the previous post, carried out until completion, titrated with TLC or other analytical method for determination of extent of reaction.

2nd reaction involves addition of aniline to the same "pot" without any purification or solvent concentration/removal.

[Anonymous No.3329558]

I'm making beer, does that count?

[Anonymous No.3329564]

Is there an infographic on how to isolate various elements?

[Anonymous No.3329589]

>>3329550


the next step is a reduction of BOTH of the unsaturated groups introduced in the previous reaction steps.

we will be reducing a styryl eneamine (reaction of phenylacetaldehyde with 4-piperidone) AND the conjugated imine (reaction of the product of previous reaction with aniline).


the product of the "sequential one-pot" previous reaction need only be concentrated and isolated from any precipitate.

Now, I should point out that because BOTH UNSATURATED GROUPS are conjugated to phenyl groups:

styryl eneamine (so essentially an amine-functionalized styrene)
n-phenyl imine

AND because we are NOT reducing carbonyl groups, we have significantly more options in terms of reduction methodology.


in fact, with the proper access to materials, THE EASIEST WAY TO DO THIS would be to reduce it in a "bomb" (high pressure metal reaction cylinder) under many atmospheres of H2 gas, in the presence of a palladium catalyst. this will reduce both of the groups to amine. Increasing the pressure only speeds up the reaction, and the reagents are relatively cheap and easy to access. Even the Pd/C is "relatively" cheap (its a catalyst, used in ~1 mol%, and very easily recovered)

alternative methods are diverse. LiBH4 would do the job.

here is a ref for catalytic hydrogenation of an eneamine (this one is conjugated to an aryl and carboxylic acid group, but it is still relevant to a single conjugation with an aryl group)
http://www.sciencedirect.com/science/article/pii/S0040403902001727

here are some alternatives for the reduction of the imine:
http://www.organic-chemistry.org/synthesis/N1H/reductionsimines.shtm

[Anonymous No.3329611]

the result of the previous step has very simple functionality:

the cyclic (6-member saturated heterocycle) core has a TERTIARY amine (unreactive under the conditions of this next step).

the amidation/reduction step has created a 2ndary amine (aniline +styryl eneamine ---> eneamine/imine (reduction)----> 2ndary amine)


the final step involves reaction with propionic anhydride/acyl chloride


this is a simple step if you use an activated reagent like the anhydride/acid chloride.

it occurs stoichiometrically, and there are no POSSIBLE side products.
again, we DID NOT purify the reaction product from the previous reduction. We simply filtered it and/or isolated any of the reduction agents (Depends on the method used)


this last step involves a simple addition of the propionic anhydride/acid chloride.


depending on the reagent used, this can be achieved "neat" in the reagent itself

Propionic anhydride is a liquid. This is the exact same reaction that a big drug producer would use to produce Heroin, but they would use acetic anhydride in place of the propionic anhydride.

[Anonymous No.3329625]

>>3329611


after this last step, we actually perform a "real" purification.


BUT: luckily we are dealing with a simple alkaloid, with SIMULTANEOUS "non polar" hydrocarbon nature.

seriously Fentanyl is the chemists dream drug.

1) nothing is overtly sensitive (oxygen, water, light, etc)

2) nothing is acid/base senstive (the only POSSIBLE exception is the "resulting" propionic AMIDE group, but as we all know AMIDES are very very unreactive)

3) purification is a snap:


the absolute ideal compound for an acid base extraction....
if dealing with super large quantities:

recrystallize repeatedly from ethanol or methanol solution (in neutral form) or from CH2Cl2/pet ether in ionic form


if dealing with smaller quantities:

chromatography.


either or. Repeated recrystallization ("fractional recrystallization) is used in the pharmaceutical industry to purify pharmaceuticals for sale to people.

[SomeStupidFag !!jgMdkqLZWtJ No.3329662]

>>3329625

thank you very much for sharing

[Anonymous No.3329668]

finally a discussion on the propionic anhydride/acid.

this is the most "watched" of all of the chemicals listed thus far... even the unmentioned possible alternative reducing/oxidizing agents used in some of the steps. depending on what you choose for your oxidizing agent: you can actually MAKE THIS YOURSELF. you would thus start with PROPENE (propylene, used to make plastic) and, in a fashion IDENTICAL to what was done with styrene: hydroboration oxidation.... followed by oxidation.

no isolation in between BUT you ABSOLUTELY MUST oxidize this ALL THE WAY to the acid.

you cannot produce an "activated carbonyl group" (like an acid chloride/bromide/iodide OR anhydride) from an aldehyde. you must start with a carboxylic acid. so your goal here would be to produce propionic acid, and then activate it: thionyl chloride, DCC, or somehow find a simple dehydrating reagent (usually these are organometallic reagents like Cobalt reagents use in carbonylation reactions). either way, the overall design of this synthesis depends on what chemicals you have access to. if you can get Propionic acid chloride/anhydride, then you would be wasting your time to do the process I just said. if, however, you have cheap easy access to a variety of oxidizing agents (for oxidizing alcohols) then you could potentially avoid "unwanted attention" by following the procedure just illustrated.

[Anonymous No.3329672]

Obviously not OP, but what are some good beginner chemistry with organic compounds?

[Anonymous No.3329674]

a simple choice of reducing agent is important for finding an easy way to reduce BOTH of the unsaturated groups introduced by the aminations. that is why I recommended the bomb-reduction. It is simple. Throw the shit in there, fill it with hydrogen, clamp down the lid.... and come back a week later and everything is done! you will also notice that the outline I gave eliminated the majority of the isolation/purification steps. many reactions are completed with side products present from previous reactions. this necessitates the use of MORE reagents for future steps (in a few instances), but purification/isolation is expensive, time consuming, and it reduces the yield.

[Anonymous No.3329919]

holy fucking jesus christ I am raging right now.


literally spent every fucking second since my last post, intricately writing up the reaction sequence I described in Chemdraw v12.


fucking got all the structures perfectly aligned, all of the arrows aligned, all of the reaction conditions nice and formatted....


go to save my file....


SHIT FUCKING CRASHES!!!!!


no temp files no wheres. Seriously pissed off right now. I am about to fucking strangle someone.

[OP !t9hZgTuuXA No.3331648]

Wow, I'm surprised to see this thread is still alive.

>>3329672
You can do a lot of chemistry starting from ethanol, methanol and isopropanol. Also, making benzene from sodium benzoate opens a lot of possibilities, like nitrobenzene (in my first post), then aniline, and also chloro- and bromobenzene.

[Anonymous No.3332097]

Hi I'm an old Swedish home chemist. I still making some experiments but most of my glass ware is used for decoration.
I think Sweden is harder than Norway for buying chemicals but its ok for buying glass.
That drug thing destroy the home chemistry for serious people. And its sad a chemistry discussions always ends ups in the drug swamp.
Same with reckless synthesis of high explosives. But carefully pyrotechnics can be a great thing. but the greatest thing is to find new paths for synthesis. One find thing is to make pure elements from minerals.
Be careful. Use goggles, gloves and common sense.

[OP !t9hZgTuuXA No.3332816]

>>3332097
Wise words.
svenskakemi.nu has a lot of chemicals, mostly pyro-related.
http://www.mamut.net/subutiken/ sells a lot of chemicals useful for the homelab, as well as nice glassware. They require that you have a company, but registering one isn't a problem. They won't ship chemicals, but visiting their shop at Stockholm University is worth the trip alone... :)
Also, Likurg.pl sells cheap, cheap reagents. Highly recommended.