Microwave (small) scale: 1-Phenyl-2-nitropropene (P2NP)

[handle]

Has anyone tried this exact recipe lately? I know Jesse_pinkman_ did a few years back. But he then went of on a Gallium tangent...

Would love to hear some experiences, lessons, tips, tweaks or tricks? Thanks all in advance.

Microwave (small) scale:
1. Benzaldehyde 100 ml, nitroethane 100 ml, glacial acetic acid 25 ml and n-butylamine 20 ml are placed into 500 ml beaker.
2. A rubber glove is put onto the beaker.
3. The beaker is put into a microwave oven.
4. The power of the microwave oven is set up on 750 W. Oven is turned on and the mixture is warmed until the boiling. The mixture is cooled down to the room temperature.
5. Step 4 is repeated several times. Minimum 6 times.
6. Next, IPA 100 ml is added, reaction mixture is stirred and put into a freezer for 12 hours. 1-Phenyl-2-nitropropene (P2NP) is crystallized.
7. The product P2NP is filtered on a Buchner funnel (suction filtration procedure), washed be a small amount of cold IPA and dried on air (or in vacuum chamber, optional).

 

[HIGGS BOSSON]

I made small amounts (up to 100g) in the microwave using this method, everything turns out quite simply.

 

[handle]

25ml GAA to 20ml amine is that best? My calculator said 40ml GAA to 20ml amine. I'll stick with 25ml unless advised otherwise.

 

[bigrob]

going to try this once supplies are here

 

[Rabidreject]

The thing is, I think I’d rather save my nitroethane for when my 3,4,5-TMOBA comes and I don’t want p2np bad enough to bother obtaining n-butylamine….but iv heard other bulky amine’s work also…would triethylamine work?

 

[Rabidreject]

Ooo that’s interesting…

I do actually plan to try and make some cyclohexylamine…

I was going to try make a video about it given there are none on YouTube - I was surprised by this tbh…if I can actually get it to work that is lol

We’ll see but if not I can just buy it in for when my 3,4,5-TMOBA comes.
I learned when I did the nitro also reaction on 2,5-DMOBA that it pays off in terms of the quantity of nitroalkane to have the correct catalyst!

Does anyone know if I could use cyclohexylamine as the catalyst for the Henry reaction of 3,4,5-TMOBA using nitroethane, so I can reduce to the corresponding TMA as well as the b-nitrostyrene intermediate for mescaline?

 

[handle]

In the freezer now. Will update with results soon. My mixture always turns a dark red colour, doesn't stay light yellow. Possible the Benzaldehyde is of lower purity? Or overheating? Or both?

 

[handle]

Not Happy with this result.

 

[BevItUp]

I don't know @handle, I think your final result looks pretty good. It's not exactly the same yellow, but I'd say it's within the range of normal deviation.
The one thing I was kind of looking at was the crystallization. In the picture they look like small squares and don't have the fiberglass look. But hey... homemade using a microwave??? Seems pretty good.

Also, the first couple look like my German Father-in-Law's homemade beer

 

[handle]

Yes, they yield was Horrific ! 10g. from 80ml NE + 80ml B + 20ml GAA + 18ml A
Pretty sure I overheated the RM on the third radiation, as it boiled and turned from the lighter color to that 'dark poly tarry color'.
It didn't help that the microwave was 1100W....
First tried 70% for 1 minute @ 770W, this was too long and to hot.
The next radiation i did at 60% for 30sec @ 660W which was too short and too cold.
The 3rd radiation was 60% for 1 minute @ 660W this was a little to long.
45 seconds @ 660W was about right, but by then it was too late, important to keep the RM at or slightly below 60c
Next time i know to start at 60% for 45 seconds @ 660W, ahhh science.