onlynikud (Stranger)
09-25-04 01:01
No 533027

BDB / "J" Synthesis

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
(Stranger)
09-26-04 15:45
No 533242

What should be done, then it is impossible for

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
09-26-04 18:08

there is probably a better way to do this
(Rated as: misinforming)

onlynikud
(Stranger)
09-30-04 15:32
No 533902

how to extract bdb

Has somebody the Monography of BDB?

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

Rhodium
(Chief Bee)
10-01-04 16:07
No 534034

Synthesis & Purificaton of BDB & MBDB

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
(Stranger)
10-19-04 00:51
No 536469

Piperonal and 1-Nitropropane method

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
(Chief Bee)
10-19-04 06:43
No 536518

Piperonal & 1-Nitropropane

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
(Stranger)
10-20-04 02:40
No 536707

Thank you very much Rhodium.

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
(Chief Bee)
10-20-04 03:20
No 536711

I think you need to UTFSE some more...

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)