Phenylacetone (P2P) synthesis from benzaldehyde with butanone

[Grubby]

Ya!ψ(｀∇´)ψThe RM after the reaction of benzaldehyde + MEK + HCI turns black and challenges the distillation of 3-Methyl-4-phenyl-3-buten-2-one with a boiling point of 269! This is the first time I bought a -60kpa vacuum pump for vacuum decompression and successfully obtained the golden yellow liquid 3-Methyl-4-phenyl-3-buten-2-one! But the machine seems to be overheated. Now I can only pause the distillation... Do you want the remaining rm to be completely distilled, right? I don’t want to distill out impurities with higher boiling points and ruin my hard work⋯

 

[Labchef]

Pls show your vacuum pump and how you used it in distillation please.

 

[Grubby]

Now looking back at the pump I used at that time, I was able to use ultra-high temperature to evaporate and distill out a product with a boiling point of 260 degrees. It was incredible. I remember that the thermometer showed about 220 degrees. You must not do what I did. I suggest you buy an oil-driven vacuum pump and test the glass interface for high-vacuum silicone. Also pay attention to safety during the application process!

 

[Kodey]

Can 3-methyl-4-phenyl-3-buten-2-one be distilled without vacuum?

 

[handle]

Apparently yes.

 

[greatwhiteshark]

How much temperature you let it heat for 95C

 

[Mo0odi]

.....
This is a video about the synthesis of phenylacetone from benzaldehyde and methyl ethyl ketone in Spanish.

Can anyone help us translate and explain this passage?

 

[methyl_man_2025]

Do you the original video with the details ?
or do you have the reaction details?
he used sulfiric acid instead of HCl gas, he also used H2O2 instead of sodium perborate.
help me please.

 

[lalalander]

Just use Oxone in 40% H2SO4. It gives 60% molar yield. I'm using this method.

 

[methyl_man_2025]

what do you mean by that?

 

[lalalander]

You add x amount of Oxone to x amount of 40% H2SO4 solution. Then, you dissolve x amount of unsaturated ketone in x amount of methanol. After that, you add the ketone+methanol solution into the H2SO4+Oxone solution and stir it at room temperature for 3 days. At the end of the reaction, you dilute the mixture with an equal volume of water and extract it with DCM and wash until neutral. And then evaporate the DCM and steam distill the crude P2P. 10 grams of Benzaldehyde+MEK crystal (unsaturated ketone) gives at least 5 grams of steam distilled P2P.

 

[The Silent Chemist]

@lalalander when you say oxone are you referring strictly to Potassium Peroxymonosulfate or the tri salt mixture of (peroxymonosulfate, bisulfate, sulfate)

I think they sell this in a 2/1/1 ratio

 

[lalalander]

Yes. I'm referring to the triple salt. Potassium Peroxymonosulfate is always available as triple salt except under very special conditions.

 

[lalalander]

Yes. I'm referring to the triple salt. Potassium Peroxymonosulfate is always available as triple salt except under very special conditions.

 

[The Silent Chemist]

Very interesting and you have clearly had success with this.
Are you willing to share some more details on this

For every gram of ketone you use

X amount of 40% H2SO4
X amount of Oxone

and you follow the Original Two Dogs write up much the same ?

I know there is more information on the vespairy but I have not been able to find it as of yet

 

[ruen]

you can turn on utomatic dabing in the options

 

[The Silent Chemist]

@lalalander Very interesting and you have clearly had success with this.

Are you willing to share some more details on this,

For every gram of ketone you use

X amount of 40% H2SO4
X amount of Oxone

and you follow the Original Two Dogs write up much the same ?

I know there is more information on the vespairy but I have not been able to find it as of yet

 

[Eleusius_hive_reboot]

THANK YOU SIR !
~~~~~~~~~~~~~~

You provided again
INFORMATION of HIGHEST VALUE

-> A Professional Crafted Write-up,
my dear Friend
___________________________________________________

I Really appreciate this whole heartedly,
i wish you all good blessings and Joy in Life !