No, it will be a different route. Acetoxy only with a peracetic acid.
Phenylacetone (P2P) synthesis from benzaldehyde with butanone
- Thread starter William D.
- Start date
Im going to try this synth with dichloro-methane (DCM). I don't see this being an issue only that it will be heavier then water. Any reason to not use readily available DCM and synth Chloroform?
Aldol Condensation.
The directions for this are in Organic Reactions
This write up seems to be more inline with what I am seeing. Has anyone actually tried to extract with solvent from the organic layer. Using chloroform won't work, as it's miscible with the organic layer. Unless I'm missing something the write up needs to be tested and modified.
Anyone tried this synth before.
The directions for this are in Organic Reactions
This write up seems to be more inline with what I am seeing. Has anyone actually tried to extract with solvent from the organic layer. Using chloroform won't work, as it's miscible with the organic layer. Unless I'm missing something the write up needs to be tested and modified.
Anyone tried this synth before.
- By TheNut22
OK. Just heat the benz-hyde and MEK with hydrochloric acid about 3-5 hours. Temp: 90-110 C.
Just thank me.
Just thank me.
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10 g benzaldehyde + 24 g MEK + 28 g hydroc.acid (~20%) = 28 g of crystals, dried in pyrex dish = 13 g of crystals.
Just keep it simple. When you are done heating, extract the brown organic layer. Wash with 40 ml of water. Extract again. Put 20 ml:s of 10% KOH-solution in. Get rid of the water. Check pH. If too acidic, or too basic, put it to 7. Get rid of the water again. Put it in freezer, because you can then, when frozen, pour the oily shit away, and get almost white crystals. Put the crystals in pyrex dish, or something and dryi it. It can liquify, but no problem. Just heat, freeze, heat, freeze, you dry those crystals, but they cannot be crispy dry. Don't know why. Maybe they are just like that.
Just keep it simple. When you are done heating, extract the brown organic layer. Wash with 40 ml of water. Extract again. Put 20 ml:s of 10% KOH-solution in. Get rid of the water. Check pH. If too acidic, or too basic, put it to 7. Get rid of the water again. Put it in freezer, because you can then, when frozen, pour the oily shit away, and get almost white crystals. Put the crystals in pyrex dish, or something and dryi it. It can liquify, but no problem. Just heat, freeze, heat, freeze, you dry those crystals, but they cannot be crispy dry. Don't know why. Maybe they are just like that.
Last edited:
- By TheNut22
But there is one odd thing. When I don't measure pH-level at all, and just put those white crystals in my measuring flask in freezer, I get double amount of pure white crystals. Today, I made almost same amount of reagents, and same way, BUT I titrated the pH-level to 7, I got just half of the crystals. I think there is something to this. Now in the evening I just put those lame 20 ml:s of crystals in freezer, and they are orange! half of it looks like might get just oil, but I just checked there is some kind of reaction between the orange solution and upper layer white crystals that have appeared in about 10 minutes. I have come to conclusion that when you do the aldol with acid and you get basic crystals and don't titrate the pH-level at all, you get double or triple amount of Methylphenylbutenone, and when it is overnight in freezer, you dump the oil in the upper layer, and thats it. So, from now on, I don't recommend the pH-level titration.
P.S I'm sorry, I made some Methcathinone today and I'm so tired, so I'm sorry for the unclear text.
Going to sleep now.
P.S I'm sorry, I made some Methcathinone today and I'm so tired, so I'm sorry for the unclear text.
Going to sleep now.
Can 3-methyl-4-phenyl-3-buten-2-one be distilled without vacuum?
- By waltjr5858
Lol it turned to some bad stuff without vac... I went on to the next step the next time with some minor cleaning and no distillation....I didn't clean up till the end with steam distillation... works fine... yield still plenty good enough. I hate the way that stuff vac distilled......
- By waltjr5858
Yup so it wasn't just me... thought I screwed something up but it's pretty easy at that point HA. I've now gotten through the entire thing and just doing a steam distillation at the end and it turns out perfectly every time. Although it took some tries to get there.
Too much GAA use maybe 1.6lish
Hydrolysis is too long in my exp
1.25eq base and 2hrs worked best for me
you didnt get 50% peroxide and attempt this
will d scale up no testing time again
Purification via methylphenylbutanones bisulfite adduct is so much superior (same with p2p) both for not having to make chloroforms sake and end purity
huge excess of mek? Intentional? also amino acids r a better cat than hcl for the aldol and id use perborate for the villiger as thats higher yielding in my exp than H2O2. Percarbonate is less good getting maybe 35% but much easier and not watched at all
Hydrolysis is too long in my exp
1.25eq base and 2hrs worked best for me
you didnt get 50% peroxide and attempt this
will d scale up no testing time againPurification via methylphenylbutanones bisulfite adduct is so much superior (same with p2p) both for not having to make chloroforms sake and end purity
huge excess of mek? Intentional? also amino acids r a better cat than hcl for the aldol and id use perborate for the villiger as thats higher yielding in my exp than H2O2. Percarbonate is less good getting maybe 35% but much easier and not watched at all
- By lalalander
I'm considering purifying P2P using bisulfite, but I've read many times that the recovery is low. What is the yield after re-liberating it from the bisulfite adduct?
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- By mewnmewamine
80s and 90s just try not to have much water in solution as bisulfite adducts are annoyingly slightly soluble in them :3
- By lalalander
Does MPB form a bisulfite adduct? No matter how many times I tried, I wasn’t successful. I tried with water, and with a methanol-water mixture. It just doesn’t work.
- By lalalander
The suspected P2P adduct was left to dry on the filter. Right now, its texture is indistinguishable from that of a mica-based eyeshadow — it looks exactly like it. Like phenylacetic acid. Is this normal?
is this route can be scaled down ?
- By mewnmewamine
Things essentially always work scaled down its scaling up where things go wrong you should be good :3