Author Topic: 2,5-DMNP via EDDA Method - some Questions  (Read 569 times)

0 Members and 1 Guest are viewing this topic.

Xicori

  • Guest
2,5-DMNP via EDDA Method - some Questions
« on: September 27, 2003, 10:08:00 AM »
High Bees!


Swim prepared EDDA as described on Rhodiums page - everything went without proplems -> nice needles of Ethylendiamine Diacetate

4,2g 2,5-DiMeO-Benzaldehyde and 0,5g EDDA were dissolved in 20ml of IPA. The IPA was heated slightly, and everything went into solution. The solution was slightly yellow colored.

Now 2,3ml of Nitroethane was added and the solution was stirred for 25 hours -> SWIM expected a dark orange/nearly blackish solution, but the color after 25 H of stirring was only a darker yellow as before with maybe a bit of orange.

The flask was set into the freezer and the contents of the flask crystallized quickly into a cake of needle-like citrus-colored yellowish crystals.

Now my question:

--> How is 2,5-DMNP supposed to look like?

--> How important is the dryness of IPA with this reaction? (Swim used 99% IPA)

When it should be darker, ill just heat up a bit to get everything again into solution, followed by another 24H of stirring.

thanks, have a nice weekebd ;)

xicori

hest

  • Guest
Re: --> How is 2,5-DMNP supposed to look...
« Reply #1 on: September 27, 2003, 11:48:00 AM »

--> How is 2,5-DMNP supposed to look like?



needle-like citrus-colored yellowish crystals


How important is the dryness of IPA with this reaction?



99% is good enough. Take a mp and a TLC, I'm sure you have yyour nitrostyrene, move on to the reduction :-)


Barium

  • Guest
Yes
« Reply #2 on: September 28, 2003, 01:09:00 PM »
As hest said, the color is right. The water content isn't so important if you look at the wet methylamine method I've posted about. 99% IPA is more than enough.