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All 9 posts Subject: BDB / "J" Synthesis Please login to post Down

onlynikud
(Stranger)
09-24-04 23:01
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[-

Ne deutsche Antwort würde ich besser verstehen.

onlynikud
(Stranger)
09-26-04 13:45
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?

Ne deutsche Antwort würde ich besser verstehen.

starlight
09-26-04 16:08
      there is probably a better way to do this
(Rated as: misinforming)

onlynikud
(Stranger)
09-30-04 13:32
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?

Ne deutsche Antwort würde ich besser verstehen.

Rhodium
(Chief Bee)
10-01-04 14:07
No 534034
User Picture       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)

^{The Hive - Clandestine Chemists Without Borders}

tryin
(Stranger)
10-18-04 22:51
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 04:43
No 536518
User Picture       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)

^{The Hive - Clandestine Chemists Without Borders}

tryin
(Stranger)
10-20-04 00:40
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 01:20
No 536711
User Picture       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)

^{The Hive - Clandestine Chemists Without Borders}

	https://the-hive.archive.erowid.org	the-hive@erowid.org



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	All 9 posts		Subject: BDB / "J" Synthesis		Please login to post		Down


		onlynikud (Stranger) 09-24-04 23:01 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[- Ne deutsche Antwort würde ich besser verstehen.



		onlynikud (Stranger) 09-26-04 13:45 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? Ne deutsche Antwort würde ich besser verstehen.



		starlight 09-26-04 16:08				there is probably a better way to do this (Rated as: misinforming)



		onlynikud (Stranger) 09-30-04 13:32 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? Ne deutsche Antwort würde ich besser verstehen.



		Rhodium (Chief Bee) 10-01-04 14:07 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) ^{The Hive - Clandestine Chemists Without Borders}



		tryin (Stranger) 10-18-04 22:51 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 04:43 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) ^{The Hive - Clandestine Chemists Without Borders}



		tryin (Stranger) 10-20-04 00:40 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 01:20 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) ^{The Hive - Clandestine Chemists Without Borders}

All 9 posts	End of thread	Top