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Author Topic: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation  (Read 251 times)

T-cowboy

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3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« on: April 17, 2013, 09:09:12 PM »
I am having trouble precipitating mdp2np.

I have done almost as in in Benzaldehyde,cyclohexylamine, nitroethane. the is however a yellow liquid. and yes i used acetid acid as in PIHKAL.

Any one got som tips for this?

thanks

transient

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #1 on: April 17, 2013, 11:36:24 PM »
I'd put it in some methanol and then in the fridge.

Electro´S

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #2 on: April 18, 2013, 01:34:41 PM »
Dissolve piperonal in nitroethane, add the ciclohexilamine (like benzaldehyde without solvent ,just with a little nitroethane excess) and proceed as always. Them put all in the freezer, It will be a yellow solid block. Try to filter out or wash the nitro-catalyst and recrystalize with Boiling IPA.
Now you are nest to ...
Also try With IPA instead of Acetic Acid.

T-cowboy

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #3 on: April 20, 2013, 04:14:04 AM »
so no dark room for weeks, just heat as benzaldehyde? and then fridge?

Electro´S

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #4 on: April 20, 2013, 05:38:17 AM »
Yes, My first attempt was not good at all, but long yellow needles was obtained.

myhero

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #5 on: April 20, 2013, 12:24:52 PM »
You can also leave it in a dark place for 3 weeks and wash the cake after breaking it with a little cold alcohol

T-cowboy

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #6 on: April 20, 2013, 11:14:56 PM »
so many ways... damn

Gypsy

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #7 on: April 21, 2013, 07:28:19 PM »
dump the lot into 10x volume cold h20

T-cowboy

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #8 on: April 23, 2013, 01:41:03 AM »
and then bisulfite? and then hydrolyze?

myhero

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #9 on: April 23, 2013, 08:48:00 AM »
man,

then just filter the damn nitropropene, if there is any and rextallize!!!

T-cowboy

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #10 on: April 23, 2013, 12:31:35 PM »
should the smell be different from the original mixture/heliotropin?

myhero

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #11 on: April 23, 2013, 01:56:14 PM »
it should be yellow

Electro´S

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #12 on: April 25, 2013, 06:33:24 PM »
Quote from: myhero on April 23, 2013, 01:56:14 PM
it should be yellow

Good point.  ;D

myhero

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #13 on: April 26, 2013, 08:29:02 AM »
I ll try posting some pictures for your reference

Sneak

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #14 on: April 26, 2013, 06:25:36 PM »
That would be great :)
If you really want to enjoy a pure, clean product the only way... is to make it yourself...

You miss 100% of the shots you don't take...

Wizard X

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #15 on: April 26, 2013, 11:57:44 PM »
1-phenyl-2-nitropropene

Molecular formula C9H9NO2
Molar mass 163.17 g mol
Appearance yellow to lemon yellow solid.
Melting point 64-66 °C.






http://www.mole-chemical.com/propanes.htm
Albert Einstein - "Great ideas often receive violent opposition from mediocre minds."

myhero

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #16 on: April 29, 2013, 08:11:37 AM »
Here 2 pics of what was done some years ago

T-cowboy

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Re: 3,4-Methylenedioxyphenyl-2-Nitropropene precipitation
« Reply #17 on: April 29, 2013, 11:19:59 AM »
thank you so much!
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