Author Topic: BDB / "J" Synthesis  (Read 2486 times)

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onlynikud

  • Guest
BDB / "J" Synthesis
« on: September 25, 2004, 01:01:00 AM »
here is the original synthesis, but in german for

2-amino-1-(3,4-methylendioxyphenyl)-butan

[upload]

https://www.the-hive.ws/forum/pic_proxie.pl/bdb.pdf?read_cache=1&update_cache=1&name=8VX0dxDXVOqAa3SYOAkFKq



I try to translate it in english:

-to a  solution of 5g (33.3 mol) of piperonal in 10 ml Nitropropan, is added 0.25 ml n-Butylamin and 0.25 ml acetic acid,

- it is heated at 140C then refluxed at this temperature  for 3h,

-it is concentrated under 60C and 1mbar

-the yielding oil is diluted under a bit heating with 7 ml Methanol

-it is cooled down at -15C and filtrated at this temperature

-add 3 ml methanol then heat it will be heated 50C and vakuum dried.

What should be done, then it is impossible for a Ghetto-Chemist to produce 1mbar

Please answer simply, and explain that non-chemist understand it[-


onlynikud

  • Guest
What should be done, then it is impossible for
« Reply #1 on: September 26, 2004, 03:45:00 PM »
What should be done, then it is impossible for a Ghetto-Chemist to produce 1mbar?

No body knows what to do, i thought here are at least a few Chemists?


starlight

  • Guest
there is probably a better way to do this
« Reply #2 on: September 26, 2004, 06:08:00 PM »

onlynikud

  • Guest
how to extract bdb
« Reply #3 on: September 30, 2004, 03:32:00 PM »
Has somebody the Monography of BDB?

Does somebody know how to clean it with a destilation or Acid/Base extraction?


Rhodium

  • Guest
Synthesis & Purificaton of BDB & MBDB
« Reply #4 on: October 01, 2004, 04:07:00 PM »

Pihkal #94 J (BDB)

(http://www.erowid.org/library/books_online/pihkal/pihkal094.shtml)

Post 443143

(Rhodium: "Synthesis of BDB/MBDB (J/Methyl-J)", Serious Chemistry)



tryin

  • Guest
Piperonal and 1-Nitropropane method
« Reply #5 on: October 19, 2004, 12:51:00 AM »
Shulgin writes that the Piperonal and 1-Nitropropane method gave "unsatisfactory yields".

I can't find the yeild results for this method anywhere. I understand that it may give yeild results Shulgin was not happy with, but for a newbee it may be worthwhile to look into.

Does anyone have the write-up for this method with results?

Rhodium

  • Guest
Piperonal & 1-Nitropropane
« Reply #6 on: October 19, 2004, 06:43:00 AM »

UTFSE for "Piperonal Nitropropane"



Post 103792

(Rhodium: "3,4-Methylenedioxyphenyl-2-nitro-1-butene", Chemistry Discourse)

Post 286086

(lugh: "HENRY CONDENSATION AT HIGH PRESSURES", Chemistry Discourse)



tryin

  • Guest
Thank you very much Rhodium.
« Reply #7 on: October 20, 2004, 02:40:00 AM »
Thank you very much Rhodium. Your knowledge never ceases to amaze me.

My question now is, could one use 3,4-Methylenedioxyphenyl-2-nitro-1-butene in place of 1-(3,4-methylenedioxyphenyl)-2-butanone in the preparation of J?

Also, how is the iron and acid reduction of the appropriate nitrostyrene carried out?

Shulgin writes:"the Efforts to prepare this ketone (I'm assuming 1-(3,4-methylenedioxyphenyl)-2-butanone)  by the iron and acid reduction of the appropriate nitrostyrene (1-(3,4-methylenedioxyphenyl)-2-nitro-1-butene, mp 64-65 °C) were thwarted by the consistently unsatisfactory yield of the precursor from the reaction between piperonal and 1-nitropropane"

Rhodium

  • Guest
I think you need to UTFSE some more...
« Reply #8 on: October 20, 2004, 03:20:00 AM »
My question now is, could one use 3,4-Methylenedioxyphenyl-2-nitro-1-butene in place of 1-(3,4-methylenedioxyphenyl)-2-butanone in the preparation of J?

Naturally. It could be reduced by any of the numerous methods available for the reduction of nitroalkenes to amines. See for example the article I linked to in my last post or

Pihkal #100 (MDA)

(http://www.erowid.org/library/books_online/pihkal/pihkal100.shtml)

Also, how is the iron and acid reduction of the appropriate nitrostyrene carried out?

See for example the preparation of MDP2P from the nitrostyrene in

Pihkal #109 (MDMA)

(http://www.erowid.org/library/books_online/pihkal/pihkal109.shtml)