Greetings,
This is my first post, I found this novel method and have not seen it shared much to date. This seems like a much easier route.
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“15g of piperonal was dissolved in 40ml of methanol under stirring in a 250ml Erlenmeyer flask. When all of the piperonal had dissolved, 7.1g nitroethane was added to the solution. The flask was put in a ice/salt-bath with magnetic stirring, and when the temperature of the solution had dropped to 0°C, an ice-cold solution of 4g of NaOH in 20ml H2O was added at such a rate that the temperature never rose above 10°C. A white precipitate formed at the bottom of the flask during this addition, which was broken up with a glass rod.
The stirring was continued for another hour, while the temperature of the solution was never allowed to rise above 5°C, and at the end of this time, 100 ml of ice-cold H2O was added to the solution, which caused even more precipitation of white solid.
The whole slurry was poured into 100 ml of ice-cold 2M HCl solution in a 500ml Erlenmeyer flask, which was gently swirled, and there was a slight bubbling and fizzing, with the color of the solution shifting from white to blue to green to yellow in under a minute. Quite spectacular! When the fizzing had subsided, the solution was once again placed in in an ice-bath with magnetic stirring.
When the temperature had dropped to about 5°C, the solution was clear with yellow granules of crude product at the bottom. The granules were filtered with suction, and recrystallized from IPA. After air-drying, the canary-yellow crystals amounted to a yield of 65-70% of theory.”
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My question to crowd source here-
If one substitute the molecular equivalent weight of piperonal for benzaldehyde will I get P2NP?
Methanol being very easy to source and no need for a catalyst. Seems in heavy basic conditions there is no need to add the catalyst when using Piperonal + Nitroethane in methanol. Once acidifying the RM crystals seem to crash out without much more effort. There are several advantages if this route works for other aldehydes.
This is my first post, I found this novel method and have not seen it shared much to date. This seems like a much easier route.
>>>>>>>Start<<<<<<<<<
“15g of piperonal was dissolved in 40ml of methanol under stirring in a 250ml Erlenmeyer flask. When all of the piperonal had dissolved, 7.1g nitroethane was added to the solution. The flask was put in a ice/salt-bath with magnetic stirring, and when the temperature of the solution had dropped to 0°C, an ice-cold solution of 4g of NaOH in 20ml H2O was added at such a rate that the temperature never rose above 10°C. A white precipitate formed at the bottom of the flask during this addition, which was broken up with a glass rod.
The stirring was continued for another hour, while the temperature of the solution was never allowed to rise above 5°C, and at the end of this time, 100 ml of ice-cold H2O was added to the solution, which caused even more precipitation of white solid.
The whole slurry was poured into 100 ml of ice-cold 2M HCl solution in a 500ml Erlenmeyer flask, which was gently swirled, and there was a slight bubbling and fizzing, with the color of the solution shifting from white to blue to green to yellow in under a minute. Quite spectacular! When the fizzing had subsided, the solution was once again placed in in an ice-bath with magnetic stirring.
When the temperature had dropped to about 5°C, the solution was clear with yellow granules of crude product at the bottom. The granules were filtered with suction, and recrystallized from IPA. After air-drying, the canary-yellow crystals amounted to a yield of 65-70% of theory.”
≥>>>>>>>>end<<<<<<<<<<
My question to crowd source here-
If one substitute the molecular equivalent weight of piperonal for benzaldehyde will I get P2NP?
Methanol being very easy to source and no need for a catalyst. Seems in heavy basic conditions there is no need to add the catalyst when using Piperonal + Nitroethane in methanol. Once acidifying the RM crystals seem to crash out without much more effort. There are several advantages if this route works for other aldehydes.
