Phenylacetone (P2P) synthesis from benzaldehyde with butanone

[MadHatter]

I guess what I'm really wondering about is the stochiometry of this reaction. In other write-ups of the bayer-williger I can't seem to find this enormous amounts of GAA. Can somebody help me with the rationale? I'm really close to trying this one out, but the amount of GAA is problematic.

 

[billythekid]

this amount of gaa is a lot and my best guess as to why is that preparing Peracetic acid in situ (during the reaction) and without a catalyst is inefficient so the chemist overcompensates to help with this, also GAA is used here as the solvent
by making the peracetic acid days before and testing the available oxygen content you are likely to get better results. This being said, I have seen professionals use this method and only get at best 35 to 65% of finished product. so an inexperienced chemist is likely to get even worse and a newbee is likely to fail or even worse hurt themselves. I recommend reading and studying and start small
make sure you thoroughly clean your finished reaction mix at the end of each step, Do not exceed -5c in the aldol condensation let mek/benzaldehyde stir overnight in the fridge after gassing.
do not exceed 60c in the Bayer villager. and research other oxidizers because I get better results with a different one.

 

[TheNut22]

My first try to do performic acid oxidation of MPB, to do it now better.
My MPB doesn't really mix to formic acid, as I put it in formic acid solution, buffered it with sodium carbonate, so
do I need a solvent for my MPB? If I do, can I use ethanol, or is acetone better? OrgUnikum? Someone? MadHatter?
I'll be VERY thankful because I don't want to mess up my reaction now, and I can give some tips for the procedure if it goes, and works well. AND, I don't have DCM... I haven't put it yet in the performic acid.

 

[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.

 

[TheNut22]

46 g benzald. (~95%) + 36.8 g MEK + 45 g hydrochloric acid (18%). 100°C to 115°C degrees.
Time: 4 hours.

I think I'll use these amounts from now on, because I've never gotten such a large organic phase, and I didn't have to put much more reagents. I was going to put all the reagents first in the same amount as before, but when I put accidentally 45 g of hydrochloric acid, even though I had to put the same 30 g. So I added more of the other reagents to the mixture as well.

The amount of MEK was proportionally less, because it ran out of it, but it didn't hurt at all, because judging by the size of the organic phase, it was a good thing. I now also heated at slightly higher temperatures. I've tried warming up also in degrees 120-130°C, but after several experiments I ended up with that degree of about 100°C. Lower temperatures reduced yields.

 

[Osmosis Vanderwaal]

I just figures the stoichometry by mol. And 31.229g of mek is =46g benzaldehyde, and when you consider the benzaldehyde is 95% you get 29.668

 

[Osmosis Vanderwaal]

and mek weighs 0.8g ml soooo 37.85ml 36.8g mek= 46MLand 46g of benzaldehyde is 48.02ml. I gotmtonget the boy on the bus, then I'll be back to finish this math problem. I'm just doing it for practice as I need to improve my chemistry math. It's even more daunting when you are switching between volume and weight, it's probably moot too, but I just want to turn it around in my head and look at it because this is probably something I will need in the future

 

[TheNut22]

46 g benzald. (~95% [43 ml]) + 36.8 g MEK (29.4 ml) + 45 g hydrochloric acid (18% [41 ml]). 100°C to 115°C degrees. Time: 4 hours. After washing: About 45 ml of crystal solution.

 

[handle]

Stage 1 completed.

 

[handle]

This is the only way a cowboy could test if he had made phenylacetone. No meth = not phenylacetone.

 

[B APPLE]

25-30 L Batch reactor with reflux condenser and heating system May I ask what this is?

 

[handle]

NO!

 

[Osmosis Vanderwaal]

It seems to be a batch reactor and a "reflux condensor", which I assume means an alihn condenser, I didn't look at the links, but those were the words

 

[Osmosis Vanderwaal]

That's some seriously red stuff. Usually the red to me is an abundance of hcl, but maybe not in this case, idk. I've found that 4:1, hcl(l) :H²SO⁴ is the equimolor amount, that uses up all of the sulfuric. Certainly 3:1 will still be gassing. Didnyou have a drying tube online with your gas?

 

[handle]

no drying tube on first attempt. will add the HCl acid directly to it next time.

 

[Osmosis Vanderwaal]

I've never tried this reaction I read it when it was posted, but not with the mind thatni was going to do it. It seems to be a lot less stressful than Glaciadates and Chinese nationals. Mek isn't watched. They cut what it can be used for so it's not on the hardware shelves anymore, but I can order it. Benzaldehyde is tough too, but I think I can can get some or synth it

 

[handle]

I will try again soon. Now I know that the 'cowboy method' does not work.

 

[Osmosis Vanderwaal]

Duh, I hadn't looked in so long. Almond extract. Imitation almond extract is water alcohol and benzaldehyde. I've read that it's often 2-3%. There is higher concentration that can be bought but it as watched

 

[handle]

Or if you can get amygdalus communis var. amara) contains three basic components, namely, benzaldehyde, glycoside amygdalin and hydrogen cyanide
Or
McCormick Almond Flavor
Water, Alcohol (32%), and Benzaldehyde.

 

[Osmosis Vanderwaal]

Guys on science madness said a certain brand was "pure benzaldehyde", Lorran Vitter almond artificial flavoring others say cassia oil is good ( cinnamon apparently

 

[handle]

I still think the Redox Reaction: Nitration of Benzyl Alcohol to Benzaldehyde" is the easiest way.

 

[Osmosis Vanderwaal]

You could be right.mwhen I was look ing for my method, I discounted it because distilling the benzl alcohol out of paint thinner was the most viable method of obtaining Benz. Alc ( the chemical companies sell it but theynprerequisite want to know too much about what you are doing with something) but I noticed recently its on Amazon, so I can just click buy and there are no questions

 

[handle]

Yeah, its strange how countries regulate chemicals.. 1 different 1 from each country.

 

[Osmosis Vanderwaal]

It's not controlled, but filling out the Sima Eldredge work sheet is daunting. WHAT college or professional licensed business are you representing what the business tax ID? What do you plan to use it for? No thanks

 

[B APPLE]

This should be a reaction kettle with reflux condensation

 

[B APPLE]

May I ask if it is necessary to separate the layers after adding distilled water in step 1 and then extract with chloroform?

 

[Osmosis Vanderwaal]

Well it is a reaction...flask. there no reflux condensor there that I see. Here i am refluxing using an erlymeyer flask and an alihn condensor, with a 110° turn-down full of magnesium sulfate as a drying tube

 

[TheNut22]

I don't understand why you gas it.