Writeup P2NP

Radiumhero · Sat Aug 20, 2005 7:43 pm

Well reading all the intresting threads in the forum swirh was animated to cook
something himselfe he just wanted to start with the everhated P2NP
so thats what he took :
benzaldehyde 44 ml
nitroethane 55 ml
butylamin 3.5ml

after mixing all well in a erlenmeyer he put the mixture on a hotplate for a still
ongoing amount of time . swirh thinks it will be about 5-6 h .

/Mixture after 1.5 h had a nice golden yellow colour
/MIxture after 3h had orange - red colour
well after everything was finished swirh put the rxn mixture in the refrigator @ ~ 2 C whereas the mixture stayed for 1 day , after this one day no changes and no xtalisation occured , so swirh fed up and put the whole stuff in the freezer @ ~ -20 C next moring swirh came to check his xtals when he saw that he didnt have some of thme he took the erlenmyer and shook the contents hard then he put it back in the freezer , when swirh came home from shopping aceton , toluol and xylol
and some washing gas ,he saw beautiful yellow xtals in the red - brown liquild
he took the flask decantet off the liquid and put the yellow xtals on some soak up
paper ... where the remaining rxn mixture ws instanly sucked in ... there the xtals are standing now , w8ing to be dry and rextalised

icecool · Insistent Chemist

SWIM found an pdf on internet it shows the synthesis of P2NP.
Due to the fear of it getting offline I uploaded it to my own server.

http://members.home.nl/icexool/P2NP.pdf

It can be downloaded here.

Radiumhero · Sun Aug 21, 2005 11:39 pm

Ye looks very nice , but after 6 h of heating my mixture had a deeper , red´-ish
colour and dindt xtalise out after putting it in the freezer @ -1 ° , well i didnt
use a deanstark due to the missin parts to build it up ( have to buy one ...)
lets see what happens to the mixture upon cooling to -20 ° ....

joe_aldehyde · huxleys associate

RH, use methylammonium acetate in methanol as catalyst. butylamine is a "dirty" catalyst, produces much crap.

nooneinparticular · Mon Aug 22, 2005 3:10 am

You might want to have a look at this Hive post:

https://www.synthetikal.com/hiveboard/methods/000419399.html

Bushroot · Sat Aug 27, 2005 3:54 pm

icecool · Insistent Chemist

SWIM used butylammonium acetate before, it really gives great yields, since the (acidic) GAA buffers the basic(alkaline) butylamine.

BTW When do you use basic in english and when do you use the word alkaline?

Radiumhero · Sat Sep 03, 2005 2:09 pm

well Swirh should try that should try that ^^
Since he wanted to know how much product hell gain when refluxing ~ 1 h
with Butylamin ( 18 ml benzaldehyde 15 ml nitroethan 4 ml butylamin )
after putting the yellow mixture in the freezer for 1 day and adding seed xtal
nothing happend well perhaps still too warm for the low yield ^^

icecool · Insistent Chemist

You should reflux it longer, or use a dean&stark trap to drive off the water since water prevents the reaction of happening.
And will give you lower yields, so if you used wet toluene or wet nitroethane then the yields are lower anyway.
To give you even better yields add equimolar GAA to the n-butylamine this will boost the yield quite a bit.

Soap · Thu Sep 08, 2005 6:50 am

the hive link mentions using nitromethane or nitroethane. with methylamine. is it possible to use nitromethane and methylamine with benzaldehyde? or is the nitroethane a must?

100 mmol of a aromatic aldehyde
105 mmol nitromethane or nitroethane
15-20 mmol methylamine as a 10-20% aqueous solution
Enough MeOH, EtOH or IPA to make the mixture stirable. Usually about 25 ml

joe_aldehyde · huxleys associate

you'll get a different product with nitromethane, are you aware of that, soap? plain benzaldehyde with nitromethane will yield something pretty useless unless you have some l-deprenyl at hand.

the alchemist · Thu Sep 08, 2005 7:08 pm

You can always evaporate off your volatiles and recrystallize the crude solids that are left behind.

icecool · Insistent Chemist

When evaporating all the volatiles the mixture will remain or start reacting again which gives you a very dirty product, better reflux it or use a dean&stark trap until the color is nicely light orange.
Then you get pure crystals, and then evaporate off the half of the remaining volume to get a 2nd crop which really needs to be reXtalized.

hAzzBEEn · Fri Sep 09, 2005 12:34 am

Radiumhero · Sat Sep 10, 2005 1:10 am

well yes since swirh tried the method with some butylaminacetat ´swirh has to admit he got 10% more yield from first xtalation what is rather nice to go on with...
Swith will take all the left over mother liqour from serveral rxn give em some more heat and fres the hell out of it ...