Phenylacetone (P2P) synthesis from benzaldehyde with butanone

[Sneaky.Base]

This method looks awesome, otc cheap chemicals.
Why expensive dcm while chloroform exists. If you want a long time coock you ll understand making chloroform is the job you have to do.
The write up method shared here is perfect, it shows it written by a professional . I ll wonder if there are any video a bout this method. Tnx for sharing this nice write up willi

 

[TheNut22]

Yes, I also support, this whole synthesis works very well.

 

[handle]

Great let's try this one.
Step 1, underway.
45g Benzaldehyde + 200ml M.E.K bubble the HCL gas from 25ml H2SO4 over 25ml Hydrochloric acid. Turned bright red in about 30mins, now stirring.

 

[handle]

Forgot a couple of steps probably will have to redo once I get a good vacuum pump, and some sodium hypochlorite for the chloroform. as I used DCM, which I'm not sure if it works or not?

 

[Labchef]

Byhyde, how do you test for neutrality? Do you test the extracted water wash for neutrality? I get no ph reading when I test the organic layer. How do I test the solution to know when it’s neutral.

 

[TheNut22]

Now that I have over 100 grams of water and acid/base -purified, but wet MPB (collected from few reactions),
I'm going to dry the crystal solution into crystals, that don't melt in room temperature. I can post a picture of that, and I can post a picture of the acetoxyphenylpropene as well, with the yields.

 

[Labchef]

TheNuts22, did you react the MPB oil with peracetic acid without distilling it or obtaining the crystalline MPB salt.

 

[handle]

Stage 1 completed.

 

[TheNut22]

You did the bubbling, did you? Do the heating with hydrochloric acid, and you'll get better results.

 

[handle]

Did the bubbling thing first and then did it again with the liquid and heating method and added them together and got a good result of MPB.
Im now on the end of STAGE 2 looking at a flask of what im guessing is 2-Acetoxy-1-phenyl-1-propene golden yellow and slightly viscous.
Eyeing up STAGE 3 now... leverage of the ester during hydrolysis..?

 

[handle]

2-acetoxy-1-phenyl-1-propene with a strong base can lead to the formation of phenylacetone and acetic acid through an elimination mechanism followed by a rearrangement. This transformation highlights the versatility of the acetoxy group in facilitating reactions that lead to the formation of ketones.

 

[handle]

Now I have this mix of phenylacetone, ethanol and DCM . 1 more step, distill the ethanol and DCM. Then maybe vacuum distill the phenylacetone.

 

[Labchef]

Handle, did you distill the MPB oil using a vacuum, if not what was your action after bubbling or heating with hcl.

 

[OrgUnikum]

160 °C is the wanted temperature in the reaction. Water can come from adding water to anhydrous formamide, using a mixture of formamide and ammonium formate (Ingersoll reagent) or by adding 85% formic acid (contains 16 % by weight water).
At 160°C the reaction will expel more water then you want removed if you do not either use a powerful condenser (Intensiv condenser with cooling mantle and coil insides) running with very cold water or you run the reaction under some pressure what raises the boiling points and you keep the water in this way.

You do not have to follow my instructions as there are none regarding the Leuckart only suggestions and warning of things which are known not to work.

I would attach some articles I find interesting but one cannot attach .pdf files anymore what makes qualified conversations here neigh to impossible.

 

[TheNut22]

Yes, I have 85% formic acid, and from ammonium formate, there comes the water, wich have to be removed. The waters that come from the formic acid and ammonium formate must be removed. That's why I use hand-warm water for 2-3 hours in the condenser. When I notice that the melted formate and P2P and other reagents or catalysts are in molten harmony with each other, I replace the condenser with ice-cold water and raise the temperature little by little, and finally to about 155-160 C when using ammonium formate. With formamide, I raise the heat faster, but steadily, and to about 165-170 C. AlCl3 has been the most reliable catalyst, at least according to the literature, and I have often succeeded in making the product up to the n-formyl derivative. I believe that everything has gone wrong when I have not been able to gasify the product, but I have tried to make it either sulfate with H2SO4 + 95% ethanol, or with hydrochloric acid + acetone. Is gassing really that important? Thanks again for the practical answer OrgUnikum!

 

[OrgUnikum]

Nobody gasses Amphetamine. The HCl salt of it is virtually unusable as it is highly hygroscopic, sucking water from the air, creating a puddle and running off.

Whats important is filtration and washing plus (steam)distillation of the base. I posted the whole post-reaction procedure already twice here I think, might be well one of my first posts on the board.

The only drug I know which lends itself to gassing is d-Meth. Already racemic meth is not good for it as it forms ultrafine crystals then which are even with vacuum not to filter, you would need a filterpress or such. Big hassle. Better titrate and evap.

 

[TheNut22]

Can you tell me if the mixer piece was the wrong size, or why it bounced around when I tried to mix? I put a new stirrer piece in the new 500ml rbf. I was preparing diphenidine from deoxybenzoin and piperidine. I'll try again because it's a really simple synthesis. At least on paper..hehh. It was my first magnetic stirrer and I messed up the settings. Now it blew the fuse, so now it's in the trash. By the way, can you advise which solvent and catalyst should be used, or should actually be used in such a reaction? As I remember, I used alcl3, and I couldn't find the whole synthesis anywhere, but I followed some patents (different compounds made from deoxybenzoin and ...). The patent concerned different analogues of diphenidine (pyrrolidine etc.)

And, thank you for your advice to Leuckart reaction! I will try it when my new heating mantle in at my door.. hehh

 

[TheNut22]

OrgUnikum: I didn't get it now. Should I use very cold water, that I use, or should I put "not-so cold" water in the condenser?
And: Should I use: That condenser that have spiral in it, or fractional column (made so it haves some shards inside), or
straight and wider condenser, or do I use my fourth condenser where it's wide, narrow, wide, narrow? Sorry I don't have the proper names of those condensers on my desk at the moment. Like everybody will notice, I'm not very experienced cooker, but I know alot of theory, and I've made couple of successfull compounds. However, my methcatinone is my bravura'. Made it many years.

 

[wael gph]

The goal of the condenser is to condense steam from the gaseous state to the liquid state. This is its mission
Very cold water improves the efficiency of the condenser
The screw condenser works well, has a longer space, and also features a screw choke

 

[TheNut22]

Wow, I didn't know that! Yes, that is the purpose on condensers. I was asking about those pressures with different condensers, because I haven't read anywhere about different pressures, but now I'm thinking yes, I think there is little bit more pressure at 160 C, with spiral condenser than of that straight, wide one.

 

[TheNut22]

wael: Do you know why they use DCM in almost every "amine" extraction, even though there is a risk that the amine-containing product will be spoiled by the chlorine in dichloromethane? Is it about the di-polarity of the solvent? If so, why not ethyl acetate rather? Bad for hydrogenations, but good for extracting amines.

I read the claim about DCM, and thought that there is always a risk of decomposition also of ethyl acetate when mixing base solutions. Chloroform would probably be better, but it's so laborious and expensive to make even the necessary quantities yourself.

DCM is pretty expensive where I live.

 

[wael gph]

don't know the truth behind that
But let me tell you that it is safe at low temperatures. They prefer it because of its low boiling point and it does not catch fire.
Perhaps chloroform is also close to it
The best is diethyl ether, but deal with it with expertise and avoid it because it causes ignition if its vapor comes into contact with an open flame.
There are safe alternatives to toluene, gasoline, hexane..

 

[wael gph]

You are good at chemistry, don't let Dcm or chloroform get the better of you
Be strong and try with the solvents available in your country
Or multiply ethanol with sulfuric acid and make a wonderful solvent. If you bring these two reagents, sulfuric acid and ethanol, raise your flag now and make diethyl ether.

 

[TheNut22]

Now I just have to tell you this. I don't want a lecture how things work in paper. I want to know how they work in real life, in real actual synthesis. I know how to do Leuckart, and I've done it about 10-15 times now. And failed, because my "P2P". Now I just don't want to fuck things up. How the condenser works is pretty annoying answer. Also if I ask the complicated, but simple to do Leuckart reaction, I don't want any lectures what is the temperature, or how to get rid of water, I know. But if you don't know the answer, please for your own respect, all of you, just say I don't know. Or is that too embarrassing? Jeesh ...

 

[Dj.Tizo]

I couldn't agree more......over the past few years I wasted thousands, on following bs advice......and Eph is banned in my country.
Just can't get the nick of making something smokeable like meth...
.or even just a amphetamine......
Not even mentioning the lab equipment....
So I couldn't agree more......
I came to sites like these to learn because I am not a chemistry qualified.....

 

[TheNut22]

Now with my new heater/stirrer, everything is going with much less hassle.
Thank you all.. be back soon..

 

[TheNut22]

Can I use anhydrous copper sulfate in the drying tube with cotton?