Microwave synthesis of P2NP

[rampage]

microwave synthesis of p2np


reagents:

50ml nitroethane,
13ml of gaa,
20ml of n-butylamine
50ml of benzaldehyde
200 ml of ipa


materials:

600watt microwave
dishwashing glove
400ml beaker
magnetic stir bar and magnetic stirrer


process:

place 50ml nitroethane, 13ml of gaa, 20ml of n-butylamine and 50ml of benzaldehyde, mixed in that order, into the beaker
allow mixture to sit for 5 minutes as the rm comes together and smoke vapour clears.
place a rubber dishwashing glove onto the beaker, i used the cheapest one available at supermarket. (do not tape glove, use appropriate size for beaker)
place rm into the microwave.

irradiate mixture on high until you see 1 to 2 bubbles rise to the surface of the beaker then stop the microwave
allow rm after each irradiation to cool to room temp, use a water bath to speed up cooling
you can use a magnetic stirrer after each irradiation while rm is cooling, this is optional.
irradiate rm 7 times.


1st irradiation

2nd irradiation

3rd irradiation

4th irradiation

5th irradiation

6th irradiation

7th irradiation

optional magnetic stirring during cool down periods

after 7 irradiations extract 1ml of the rm and allow to evaporate and form a seed crystal

add 200ml of ipa to rm

add seed crystal

crystallisation should happen very quickly

cover beaker with glad wrap and place into the freezer

remove from freezer once crystallisation is complete this can take several hrs

vacuum filter rm and wash with cold ipa

place motherliquour back into freezer for a second crop


air dry product

yield 70gms dry weight p2np

 

[handle]

Fantastic work! seems like an excellent yield too!!

 

[thegenuinechem]

Great work friend

 

[w2x3f5]

I recommend thoroughly rinsing the finished P2NP and then re-crystallizing it in IPA. This will seriously reduce the admixture of amine acetate and reduce the amount of admixtures from side reactions in P2NP. Too much butylamine was used, 10 percent of amine acetate from the equivalent of benzaldehyde is enough for this reaction. The glass should be reduced so that there is less oxygen inside, or internal gas inside

 

[rampage]

thanks for your comments i will try less n-butylamine next time and a smaller beaker

 

[orphan]

Is the 600w microwave more of a suggestion, or a hard limit? Would yield/purity be affected if the wattage was boosted to 700w or more?

 

[rampage]

600w is all i have, so you can use a higher wattage microwave, just stop it as soon as you see a couples of bubbles rise to the surface of the rm

 

[w2x3f5]

more power, faster heating, nitroethane can boil. in my practice it once caught fire with a blue flame. the glove on the flask burned through and the nitroethane vapor caught fire with a blue flame in the neck of the flask. The total number of watts per mole is important and take into account that some of the radiation is lost.