Yep!
I Had read a lot of times this thread on SM, And I have found some numbers on the work of Stoichiometric_Steve.
http://www.sciencemadness.org/talk/viewthread.php?tid=4965
Items:
15L. Plastic Box.
Small water pump
5L Beaker.
Motor head from a 12V Drill.
Variable power supply for the drill.
Stirrer rod made with a computer fan.
Hot Plate.
Reagents:
25gr -P2NP (Recovered from a "Dungeon Waters Bottle"
12,5gr NaBH4.
250 ml Denatured ethanol bottle.
Some water.
Some Acetic Acid
Some concentrated HCl
100 gr Zinc Dust "activated"
45 gr Ammonium Formate.
The 5L beaker is place in the plastic box with cold water and the small pump recirculating it around the glass. Then a 250 ml Ethanol bottle is open with the mouth and the liquid is place in the beaker with 50-100 ml H2O and 12,5 gr NaBH4 with vigorous stirring.
Then the 25 gr of P2NP is added in 3 portions in less than ONE MINUTE. High hydrogen evolution is observed but the flask is big enough. The solution is stirrer for half hour around.
At this point, some Acetic acid is used to kill borohydride and made the precipitate a little soluble in the liquid phase.
While 100gr of zinc was activated and it was just drain off and added to the nitroalkane mixture. Reaction start a this point for the acid traces on the zinc, and the ammonium formate is drop down in 3 portions in less than one minute. All was stirrer for 15 minutes.
Now water bath and stirrer is removed and the beaker is place on the hot plate and 200 ml of concentrated HCl is added in portions. The beaker was heated and stirred with a glass rod for 30-40 minutes. And the reaction was finished at this point.
After basification, extraction, boiling out the ammonia, drying the solvent y neutralization... 24 grams of the propylamine sulfate was obtained.
So looks like the Stoichiometric_Steve procedure works perfectly for Nitropropene even if you make it with not too much attention.
I Had read a lot of times this thread on SM, And I have found some numbers on the work of Stoichiometric_Steve.
http://www.sciencemadness.org/talk/viewthread.php?tid=4965
Items:
15L. Plastic Box.
Small water pump
5L Beaker.
Motor head from a 12V Drill.
Variable power supply for the drill.
Stirrer rod made with a computer fan.
Hot Plate.
Reagents:
25gr -P2NP (Recovered from a "Dungeon Waters Bottle"
12,5gr NaBH4.
250 ml Denatured ethanol bottle.
Some water.
Some Acetic Acid
Some concentrated HCl
100 gr Zinc Dust "activated"
45 gr Ammonium Formate.
The 5L beaker is place in the plastic box with cold water and the small pump recirculating it around the glass. Then a 250 ml Ethanol bottle is open with the mouth and the liquid is place in the beaker with 50-100 ml H2O and 12,5 gr NaBH4 with vigorous stirring.
Then the 25 gr of P2NP is added in 3 portions in less than ONE MINUTE. High hydrogen evolution is observed but the flask is big enough. The solution is stirrer for half hour around.
At this point, some Acetic acid is used to kill borohydride and made the precipitate a little soluble in the liquid phase.
While 100gr of zinc was activated and it was just drain off and added to the nitroalkane mixture. Reaction start a this point for the acid traces on the zinc, and the ammonium formate is drop down in 3 portions in less than one minute. All was stirrer for 15 minutes.
Now water bath and stirrer is removed and the beaker is place on the hot plate and 200 ml of concentrated HCl is added in portions. The beaker was heated and stirred with a glass rod for 30-40 minutes. And the reaction was finished at this point.
After basification, extraction, boiling out the ammonia, drying the solvent y neutralization... 24 grams of the propylamine sulfate was obtained.

So looks like the Stoichiometric_Steve procedure works perfectly for Nitropropene even if you make it with not too much attention.

