Author Topic: Preperation of 2,5dimethoxyphenyl-2-nitropropene  (Read 4860 times)

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Barium

  • Guest
Suggestion
« Reply #20 on: March 11, 2003, 11:04:00 AM »
It seems like you had some nitrostyrene at least. After the reduction to the nitroalkane try the KCOOH/Pd-C CTH in IPA. It should work like a charm. For saftys sake don´t stress the nitroalkane like that by subjecting it to such high temps like you did last time. I know they should be able to handle those temps but it´s advisable not to push the luck.


starlight

  • Guest
did you recrystallize the nitropropene
« Reply #21 on: March 11, 2003, 12:00:00 PM »
before reducing it?

i have heard of problems similar to this when the starting nitropropene was not sufficiently pure.

Antibody2

  • Guest
the NaBH4 rxn is very water sensitive, you...
« Reply #22 on: March 12, 2003, 12:34:00 AM »
the NaBH4 rxn is very water sensitive, you mention using EtOH. was it anhydrous EtOH or did you dry your solvents first, you didn't mention anything about drying?

you have to be obessive/compulsive about drying the reagents for that rxn, seriously or else ::)  :(

Vibrating_Lights

  • Guest
THF
« Reply #23 on: March 12, 2003, 03:04:00 AM »
THF is going to be used next.  I first need to find out if the nitropropene synth is good.  I will make the nitropropene with AmmAcOH then reduce with NaBH4 in THF.  I need to compare the nitropropene to a standard synth.
VL_


Antibody2

  • Guest
the NaOH/MeOH condensation its a good rxn.
« Reply #24 on: March 12, 2003, 05:20:00 PM »
the NaOH/MeOH condensation its a good rxn. Why don't you simply take a MP of the nitro and you wil know whether or not its any good. I expect your trouble is coming from the NaBH4 rxn. IPA or dry EtOH is what you want to use.

Vibrating_Lights

  • Guest
honestly
« Reply #25 on: March 12, 2003, 09:47:00 PM »
I don't  have a fucking thermometer.  I gave all my shit to someone and it got seized.  I hope the new shit gets here soon
vl_


foxy2

  • Guest
I don't have a fucking thermometer.
« Reply #26 on: March 12, 2003, 10:23:00 PM »
I don't  have a fucking thermometer.  I gave all my shit to someone and it got seized.  I hope the new shit gets here soon

Yea that sounds like the ideal situation to start cooking again.  ::)

Vibrating_Lights

  • Guest
learned
« Reply #27 on: March 12, 2003, 10:34:00 PM »
I learned how to cook with Pots and Pans blind.  Then I had a goard of materials to work with.  Now that i have pots and pans again i really know how to use them.  Granted a thermometer is important, But the most meaningful product will always come from pots and pans(nonstick of course). Oh and I hand stirr with a teflon spatchula for hours at a time.  Now thats dedicaton.  Damn pussies with your electrik stirrplates, born with a silver stirbar in your mouth. Once I get this down I'll stirr the bucket with a plunger handle. Keep that shit real. There is no love involved in turning a switch.
HeeHaw
VL_


Antibody2

  • Guest
OMG!
« Reply #28 on: March 12, 2003, 10:51:00 PM »
:o

Vibrating_Lights

  • Guest
HeeHaw
« Reply #29 on: March 12, 2003, 11:06:00 PM »
;)


weedar

  • Guest
That's impressive
« Reply #30 on: March 13, 2003, 05:51:00 PM »
You don't lack any dedication.

I was just waiting for you to write:
"I told u I was hardcore" ;)