Benzaldehyde and MEK - TwoDogs Method

[BayHyde]

When 10 grams of Benzaldehyde + 10 grams of MEK and 7 grams of 30.5% aqueous HCl are mixed for 24 hours at room temperature, I obtain an organic layer.

The reaction should be carried out in an inert reactor, and the mouth of the reactor should be sealed with an inert stopper (such as LDPE, Teflon, glass, etc.).

I wash the organic layer with NaHCO3 solution until it is neutral and put it directly into the freezer. No heating. I filter it using a vacuum cleaner motor. This separates the remaining residual Benzaldehyde and MEK. White crystals remains behind.

When I pour -18 degree methanol on it, I obtain completely snow-white crystals. In my last test, I used 50 grams of Benzaldehyde + 50 grams of MEK and 35 grams of 30.5% aqueous HCl. I obtained 46 grams of snow-white crystals.

Methanol must be cooled in the freezer. Otherwise a lot of crystal will dissolve in the washing step.

I also think you can use ice water when washing, but I haven't tried it yet.

I no longer have any problem with aldol condensation step.

Here is a picture showing the upper organic layer, the lower aqueous layer, and the crystals obtained after freezing, before washing with cold methanol, for anyone is interested;

 

[lalalander]

When 10 grams of Benzaldehyde + 10 grams of MEK and 7 grams of 30.5% aqueous HCl are mixed for 24 hours at room temperature, I obtain an organic layer.

The reaction should be carried out in an inert reactor, and the mouth of the reactor should be sealed with an inert stopper (such as LDPE, Teflon, glass, etc.).

I wash the organic layer with NaHCO3 solution until it is neutral and put it directly into the freezer. No heating. I filter it using a vacuum cleaner motor. This separates the remaining residual Benzaldehyde and MEK. White crystals remains behind.

When I pour -18 degree methanol on it, I obtain completely snow-white crystals. In my last test, I used 50 grams of Benzaldehyde + 50 grams of MEK and 35 grams of 30.5% aqueous HCl. I obtained 46 grams of snow-white crystals.

Methanol must be cooled in the freezer. Otherwise a lot of crystal will dissolve in the washing step.

I also think you can use ice water when washing, but I haven't tried it yet.

I no longer have any problem with aldol condensation step.

Here is a picture showing the upper organic layer, the lower aqueous layer, and the crystals obtained after freezing, before washing with cold methanol, for anyone is interested;

 

[chema12]

Hola amigo

 

[Newbee]

can anybody provide me receipt to it

• lalalander

 

[lalalander]

When 10 grams of Benzaldehyde + 10 grams of MEK and 7 grams of 30.5% aqueous HCl are mixed for 24 hours at room temperature, I obtain an organic layer.

The reaction should be carried out in an inert reactor, and the mouth of the reactor should be sealed with an inert stopper (such as LDPE, Teflon, glass, etc.).

I wash the organic layer with NaHCO3 solution until it is neutral and put it directly into the freezer. No heating. I filter it using a vacuum cleaner motor. This separates the remaining residual Benzaldehyde and MEK. White crystals remains behind.

When I pour -18 degree methanol on it, I obtain completely snow-white crystals. In my last test, I used 50 grams of Benzaldehyde + 50 grams of MEK and 35 grams of 30.5% aqueous HCl. I obtained 46 grams of snow-white crystals.

Methanol must be cooled in the freezer. Otherwise a lot of crystal will dissolve in the washing step.

I also think you can use ice water when washing, but I haven't tried it yet.

 

[lalalander]

My "P2P" smells very much like "burnt" benzaldehyde. After a while it starts to resemble apple flavor. There is also a very light honey note. But it smells predominantly like burnt benzaldehyde. And it takes hours to steam distill any usable amount. If I hydrolyze the ester separately with NaOH solution, a very dominant methyl acetate smell is emitted from the mixture.

 

[LabPsycho]

I just wash the ester solution 2 times with water, and the acetic acid smell is gone.

 

[AKINCI]

How does it become P2P?

 

[LabPsycho]

I'm little bit confused. Are you asking me? If you are, what "it"? And if you are talking about acetoxyphenylpropene, don't ask from me because like you see, people get also confused. Confused from the smell of phenylpropanone.

 

[LabPsycho]

What I mean, is not to be an ass. I have just seen very weird questions lately. Like how do you make a compound from a to b to c, when the whole procedure is known in here, or at least written the whole synthesis procedure in here! All I can say for those kind of ... weirdness is that I don't know shit about nothing.

 

[lalalander]

Instead of asking non-specific questions like the village lunatic to everyone who comes by, go and do some literature research. You're getting annoying. No one is going to teach you things step by step. If that's your expectation, don't bother waiting. Everyone puts in effort, and no one is willing to teach someone who doesn't even bother to read. You keep asking same question after another even when the answers are clearly given.

 

[lalalander]

Hey, LabPshyco. Can you kindly share the ratios you use for performic acid?

 

[LabPsycho]

I don't just understand where did you get the impression that I was asking anything here...?

 

[LabPsycho]

 

[LabPsycho]

Like I have said before, of course I'll help you, or someone else with synthesis problems, if I can help, but if the question is can you please tell me how much you made something/anything this week, all I can say, nada. Giving you the yield from some compound will actually help you?! Please ...

 

[lalalander]

"I don't just understand where did you get the impression that I was asking anything here...?"

That reply was for AKINCI. He constantly asks something but never reads the answers and keeps asking the same thing.

 

[Osmosis Vanderwaal]

Wow, a loot of responses here. I forgot that I responded, but I should have added, if your alihn condensor isn't gtting the job done, put your lieberman condensor first and your align on top of that and run a little piece of hose from the top of the bttom to the bottom of the top ("daiy-chain" them") also if your not using ice in your condensor water, you should (I run my pump in the bucket that my recieving flask is in, so that cools the flask and the condensor water) don't know if anone suggested that

 

[lalalander]

I diluted the HCl to 15%. There is no more HCl gas escaping, but this is no longer necessary. I carry out the aldol condensation at room temperature.

 

[LabPsycho]

I can only say that if such behavior is allowed by the moderators, then even though I know that there are no illegal molecules or equipment for their production near me, I will stay away from this page and will share my knowledge. Because you ask different steps of the synthesis again and again from different users here, even though I assumed that you realize the stupidity of your talk yourself. What do you think, why am I not surprised?

I'm not a chemist. Just an actor, so I don't know.

 

[LabPsycho]

I mean that post to lalalander.

 

[onedeepnz]

What does it mean if I’m getting rings setting very slowly at end of reductive amination of p2p made via two dogs method. I’m guessing it because Of a incomplete reaction?

 

[lalalander]

Can you elaborate?

 

[onedeepnz]

The product that I end up with after reduction is like pinwheels and takes a long time to set. Looks like spider webs or pinwheels and I’m unsure what is going wrong. I’ve done this about 10 times with same result weather I use iso or methanol