Phenylacetone (P2P) synthesis from benzaldehyde with butanone

[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]

FAILED ATTEMPT, probably failed at stage 2! As I used 49% acetic acid and not glacial.

No precipitation.

 

[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.

 

[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.