How about final fractional destillation of the last filtrate? Any possibility to recover unreacted viable nitroethane? It's really precious these days ...
More for curiosity, When looking a nitroaldol/Henry reaction i notice that the carbonyl gets reduced only once and stays, somehow with our reaction, the P2NP is made without there being a hydroxy group anywhere.... Is this because we used a mild base, cyclohexylamine/n-butylamine instead of NaOH? Does that somehow reduce it all the way?
Also, can MeOH be used instead of GAA? I can get GAA, but methanol can be found at any gas station....
Still curious is sodium methoxide can be used as the base or if that's only with certain styrenes? I've been unable to find any mention of it. Also, many years ago I used Diphenylamime and got an amazing yield. Unfortunately I can't recall any of the conditions or the exact styrene that was being produced. I do remember being surprised be the outcome. Same with no mention of it anywhere..
After P2NP crystallized out you shall distill off 60% from the liquids left over, add 1 gr crystall P2NP into it, put in freezer and another 5-8% of P2NP will crystallize out from that (little darker, need to be re-crystallized 2x). P2NP shall always be washed with sodium bisulphite to rinse out contamination of benzaldehyde, the benzaldehyde interfere in whatever method you had in mind for your P2NP. A 6-8% solution sodium bisulphite in water wash out all benzaldehyde contaminatioon from the P2NP.
Running this reaction in an ultrasonic bath instead of reflux give better yield with less than half time work. 2.5 hrs US power at 40-45 KHz. Methylamine in dry MeOH instead of GGA + cyclohexylamine gives higher yield. Try it and you'll see guys.
My synthesis: 1M benzaldehyde, 1.1M nitroethan, 0.1M methylamine in 600 ml dry methanol. Let stand in darkness 2 wks and you hit minimum 75-79% yield, after 3 wks 83-87%. If you don't like waiting that long, run it in ultrasonic power 2.5 hrs and you'll have 7-10% less yield. Standing 3-4 wks in darkness give highest & cleanest yield every single time
I wanted to ask a question in this video in the description one reagent is quite tight as well as in the video it is not cyclohexamine to what they adhere to since the description is written either as in the video or you can make a video full video how to start synthesize p2np and then how to synthesize amphetamine thank you
More for curiosity, When looking a nitroaldol/Henry reaction i notice that the carbonyl gets reduced only once and stays, somehow with our reaction, the P2NP is made without there being a hydroxy group anywhere.... Is this because we used a mild base, cyclohexylamine/n-butylamine instead of NaOH? Does that somehow reduce it all the way?
Genuine question, if SWIM replaces the cyclohexylamine with n-butylamine, should he use the same amount/ratio shown in the video? Also, many people use Ethanol or Methanol instead of GAA, so would that be viable?
I do not know if I can link videos but there is one on youtube with n-butylamine and Ethanol and it seems to work.
Thanks
After P2NP crystallized out you shall distill off 60% from the liquids left over, add 1 gr crystall P2NP into it, put in freezer and another 5-8% of P2NP will crystallize out from that (little darker, need to be re-crystallized 2x). P2NP shall always be washed with sodium bisulphite to rinse out contamination of benzaldehyde, the benzaldehyde interfere in whatever method you had in mind for your P2NP. A 6-8% solution sodium bisulphite in water wash out all benzaldehyde contaminatioon from the P2NP.
Running this reaction in an ultrasonic bath instead of reflux give better yield with less than half time work. 2.5 hrs US power at 40-45 KHz. Methylamine in dry MeOH instead of GGA + cyclohexylamine gives higher yield. Try it and you'll see guys.
My synthesis: 1M benzaldehyde, 1.1M nitroethan, 0.1M methylamine in 600 ml dry methanol. Let stand in darkness 2 wks and you hit minimum 75-79% yield, after 3 wks 83-87%. If you don't like waiting that longer , run it in ultrasonic power 2.5 hrs and you'll have 7-10% less yield. Standing 3-4 wks in darkness give highest & cleanest yield every single time
Could you write up a work up on your preparation of the methyllamine in MeOH? I’m assuming SWIY synthesized methlyamine hcl and then freebased it w KOH or NaOH? I think I read somewhere that KOH was more readily soluble in methanol.
After P2NP crystallized out you shall distill off 60% from the liquids left over, add 1 gr crystall P2NP into it, put in freezer and another 5-8% of P2NP will crystallize out from that (little darker, need to be re-crystallized 2x). P2NP shall always be washed with sodium bisulphite to rinse out contamination of benzaldehyde, the benzaldehyde interfere in whatever method you had in mind for your P2NP. A 6-8% solution sodium bisulphite in water wash out all benzaldehyde contaminatioon from the P2NP.
Running this reaction in an ultrasonic bath instead of reflux give better yield with less than half time work. 2.5 hrs US power at 40-45 KHz. Methylamine in dry MeOH instead of GGA + cyclohexylamine gives higher yield. Try it and you'll see guys.
My synthesis: 1M benzaldehyde, 1.1M nitroethan, 0.1M methylamine in 600 ml dry methanol. Let stand in darkness 2 wks and you hit minimum 75-79% yield, after 3 wks 83-87%. If you don't like waiting that long, run it in ultrasonic power 2.5 hrs and you'll have 7-10% less yield. Standing 3-4 wks in darkness give highest & cleanest yield every single time
More for curiosity, When looking a nitroaldol/Henry reaction i notice that the carbonyl gets reduced only once and stays, somehow with our reaction, the P2NP is made without there being a hydroxy group anywhere.... Is this because we used a mild base, cyclohexylamine/n-butylamine instead of NaOH? Does that somehow reduce it all the way?
Also, can MeOH be used instead of GAA? I can get GAA, but methanol can be found at any gas station....
It's a different thing when NaOH is employed as catalyst, for example the nitroalkene is formed when a thin stream of reaction mixture is poured into ice and dilute HCl as it precipitates. It is said that pouring the acid into the reaction mixture will result in the formation of the nitro alcohol that must be vacuum distilled as it is of that low purity it's pretty much useless.
Is anyone else having issues downloading the video. It seems to download at a snails pace and ends up just failing. Is there anything I can do on my end to make it download without failing? Excellent work by the way and thank you for your efforts with these videos.
The servers here seem to be hitting capacity most of the time or have a huge latency issue, it’s hard to
Get most of the bigger videos to complete a download.
There are mirrors of a lot of these videos on YouTube. Some of them are available for download straight from YouTube with a download button if you have a premium account. Or you can use something like the Video Download Helper plugin on your browser.
P2np synth mirror is here at the moment (will probably get deleted eventually) https://youtu(.)be/JqLjbmsJyPk?si=Mq6MW3AStqwSmlTV
My reaction won't go. I used 20ml Cyclohexylamine (99.5+%, <0.3% H2O), 100ml Benzaldehyde (99.8%, Pure, FCC, Food grade), 40ml GAA (99.8-100.5+%) and 100ml Nitroethane that I distilled from Acrifix 1S 0117 solvent based adhesive. I don't think I got rid of the Butan-1-ol (1-<3%, BP 117.7 C) it's contaminated with. Not 100% sure about the ethyl acetate (3-7%, BP 77.1 C). Could contamination be the problem and what should I do guys!? It's been sitting in water bath at 60 C for over 6h now and the Rm is the same clear light yellow as in beginning.
My reaction won't go. I used 20ml Cyclohexylamine (99.5+%, <0.3% H2O), 100ml Benzaldehyde (99.8%, Pure, FCC, Food grade), 40ml GAA (99.8-100.5+%) and 100ml Nitroethane that I distilled from Acrifix 1S 0117 solvent based adhesive. I don't think I got rid of the Butan-1-ol (1-<3%, BP 117.7 C) it's contaminated with. Not 100% sure about the ethyl acetate (3-7%, BP 77.1 C). Could contamination be the problem and what should I do guys!? It's been sitting in water bath at 60 C for over 6h now and the Rm is the same clear light yellow as in beginning.
Couldn't log in for long time. The reaction went! After 6h at 60 C bath I rised the temperature to 100 C. The solution turned clear reddish and I kept it in bath for another 5h. About 6h after taking it out I noticed it had turned cloudy. Another 5 hours and the layers had separated. I wondered if it would ever crystallise and when separating the layers in the funnel, Hallelujah it went solid!
The servers here seem to be hitting capacity most of the time or have a huge latency issue, it’s hard to
Get most of the bigger videos to complete a download.
There are mirrors of a lot of these videos on YouTube. Some of them are available for download straight from YouTube with a download button if you have a premium account. Or you can use something like the Video Download Helper plugin on your browser.
P2np synth mirror is here at the moment (will probably get deleted eventually) https://youtu(.)be/JqLjbmsJyPk?si=Mq6MW3AStqwSmlTV
i dont understand thay wrote benzaldehyde 1000 ml.nitroethane 1000 ml.Acetic acid 250ml and n-butalamine only 50 ml. And in this vedio nitroethane and benzaldehyde 750 and 750, acetic acid 300ml and cyclohexalamine 150? Is PH dosenot matter? Haw base work? Anyone halp me plz
Couldn't log in for long time. The reaction went! After 6h at 60 C bath I rised the temperature to 100 C. The solution turned clear reddish and I kept it in bath for another 5h. About 6h after taking it out I noticed it had turned cloudy. Another 5 hours and the layers had separated. I wondered if it would ever crystallise and when separating the layers in the funnel, Hallelujah it went solid!
