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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 (https://www.thevespiary.org/rhodium/Rhodium/hive/hiveboard/picproxie_docs/000533027-bdb.pdf)
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[-
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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?
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Has somebody the Monography of BDB?
Does somebody know how to clean it with a destilation or Acid/Base extraction?
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Pihkal #94 J (BDB) (http://www.erowid.org/library/books_online/pihkal/pihkal094.shtml)
(http://www.erowid.org/library/books_online/pihkal/pihkal094.shtml)
Post 443143 (https://www.thevespiary.org/talk/index.php?topic=12542.msg44314300#msg44314300)
(Rhodium: "Synthesis of BDB/MBDB (J/Methyl-J)", Serious Chemistry)
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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?
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UTFSE for "Piperonal Nitropropane" (https://www.the-hive.ws/forum/search.pl?Cat=&All_Forums=on&Text_simple=Piperonal%20Nitropropane&Preview=on&RatePlus=on&RateNeutral=on&Search_simple=on)
Post 103792 (https://www.thevespiary.org/talk/index.php?topic=7493.msg10379200#msg10379200)
(Rhodium: "3,4-Methylenedioxyphenyl-2-nitro-1-butene", Chemistry Discourse)
Post 286086 (https://www.thevespiary.org/talk/index.php?topic=7680.msg28608600#msg28608600)
(lugh: "HENRY CONDENSATION AT HIGH PRESSURES", Chemistry Discourse)
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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"
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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)
(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)
(http://www.erowid.org/library/books_online/pihkal/pihkal109.shtml)