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All 7 posts Subject: Pihkal #100 MDA Please login to post Down

lastchance
(Stranger)
04-13-04 12:42
No 500560
      Pihkal #100 MDA

Accordiong to Shulgin the following synthesis looks pretty easy. Any hints on betttering the yields or unforseen dangers. Also why did he through in theh MDP2P Synth if the first part is complete?
SYNTHESIS: (from piperonal) To a solution of 15.0 g piperonal in 80 mL glacial acetic acid there was added 15 mL nitroethane followed by 10 g cyclohexylamine. The mixture was held at steam-bath temperature for 6 h, diluted with 10 mL H2O, seeded with a crystal of product, and cooled overnight at 10 °C. The bright yellow crystals were removed by filtration, and air dried to yield 10.7 g of 1-(3,4-methylenedioxyphenyl)-2-nitropropene with a mp of 93-94 °C. This was raised to 97-98 °C by recrystallization from acetic acid. The more conventional efforts of nitrostyrene synthesis using an excess of nitroethane as a solvent and anhydrous ammonium acetate as the base, gives impure product in very poor yields. The nitrostyrene has been successfully made from the components in cold MeOH, with aqueous NaOH as the base.

A suspension of 20 g LAH in 250 mL anhydrous THF was placed under an inert atmosphere and stirred magnetically. There was added, dropwise, 18 g of 1-(3,4-methylenedioxyphenyl)-2-nitropropene in solution in THF and the reaction mixture was maintained at reflux for 36 h. After being brought back to room temperature, the excess hydride was destroyed with 15 mL IPA, followed by 15 mL of 15% NaOH (Also is Red Devil Lye ok yo substitute for NAOH). An additional 50 mL H2O was added to complete the conversion of the aluminum salts to a loose, white, easily filtered solid. This was removed by filtration, and the filter cake washed with additional THF. The combined filtrate and washes were stripped of solvent under vacuum, and the residue dissolved in dilute H2SO4. Washing with 3x75 mL CH2Cl2 removed much of the color, and the aqueous phase was made basic and reextracted with 3x100 mL CH2Cl2 (Methylene Chloride). Removal of the solvent yielded 13.0 g of a yellow-colored oil that was distilled. The fraction boiling at 80-90 °C at 0.2 mm weighed 10.2 g and was water-white. It was dissolved in 60 mL of IPA (Is 91% store bought ok), neutralization with concentrated HCl, and diluted with 120 mL of anhydrous Et2O (Is DCM ok to substitute)which produced a lasting turbidity. Crystals formed spontaneously which were removed by filtration, washed with Et2O, and air dried to provide 10.4 g of 3,4-methylenedioxyamphetamine hydrochloride (MDA) with a mp of 187-188 °C.

[b]

hypo
(Hive Addict)
04-13-04 12:51
No 500562
      no problem...

if you have access to LAH and nitroethane, that is. tongue

http://www.google.com/search?q=millenium

Sunlight
(Pioneer Researcher)
04-13-04 23:43
No 500684
      And piperonal

Don't forget the aldehyde.

amine
(Hive Bee)
04-16-04 19:22
No 501107
      If you can get safrole you can look into this...

If you can get safrole you can look into this route:

Safrole to Isosafrole (via Isomerization)
Isosafrole to MDP2P (via Performic/Oxone/Peracetic use HCL for hydrolysis)
MDP2P to the Oxime.
Al/Hg reduction of the oxime.
:)
MDA

Its all there on rhodiums MDMA page.
if u need links pm me.

lastchance
(Stranger)
04-19-04 23:51
No 501685
      Al/Hg reduction of the oxime. is stupid

SWIM has done hundreds of reactions converting MDP2P tp MDA but would never consider AL/HG it is very dangerous to the environment. I spelt a little in my back yard and after 2 years nothing would grow there. Sodium Cyano is much better. My question is the first part of PIHKAL MDA complete? I am not a morone and I think it is I just wanted some one ike Rohodium to confirm it.   I sure do miss Strike.

Barium
(Heavyweight Chempion(eer))
04-20-04 09:06
No 501753
      If you know what you are doing Al(Hg) is not...

If you know what you are doing Al(Hg) is not enviromentally dangereous since the mercury is easy to recover.

Sunlight
(Pioneer Researcher)
04-20-04 23:13
No 501887
      MDA by CTH reductive amination

I believe is the best method if you can get Pd/C and ammonium formate. 70-80 % yeild using 20-30 % of 10 % catalyst, and washing it with NaOH solution extensively and then with water till pH 7 it works 5-7 times. UTFSE.

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	All 7 posts		Subject: Pihkal #100 MDA		Please login to post		Down


		lastchance (Stranger) 04-13-04 12:42 No 500560				Pihkal #100 MDA
						Accordiong to Shulgin the following synthesis looks pretty easy. Any hints on betttering the yields or unforseen dangers. Also why did he through in theh MDP2P Synth if the first part is complete? SYNTHESIS: (from piperonal) To a solution of 15.0 g piperonal in 80 mL glacial acetic acid there was added 15 mL nitroethane followed by 10 g cyclohexylamine. The mixture was held at steam-bath temperature for 6 h, diluted with 10 mL H2O, seeded with a crystal of product, and cooled overnight at 10 °C. The bright yellow crystals were removed by filtration, and air dried to yield 10.7 g of 1-(3,4-methylenedioxyphenyl)-2-nitropropene with a mp of 93-94 °C. This was raised to 97-98 °C by recrystallization from acetic acid. The more conventional efforts of nitrostyrene synthesis using an excess of nitroethane as a solvent and anhydrous ammonium acetate as the base, gives impure product in very poor yields. The nitrostyrene has been successfully made from the components in cold MeOH, with aqueous NaOH as the base. A suspension of 20 g LAH in 250 mL anhydrous THF was placed under an inert atmosphere and stirred magnetically. There was added, dropwise, 18 g of 1-(3,4-methylenedioxyphenyl)-2-nitropropene in solution in THF and the reaction mixture was maintained at reflux for 36 h. After being brought back to room temperature, the excess hydride was destroyed with 15 mL IPA, followed by 15 mL of 15% NaOH (Also is Red Devil Lye ok yo substitute for NAOH). An additional 50 mL H2O was added to complete the conversion of the aluminum salts to a loose, white, easily filtered solid. This was removed by filtration, and the filter cake washed with additional THF. The combined filtrate and washes were stripped of solvent under vacuum, and the residue dissolved in dilute H2SO4. Washing with 3x75 mL CH2Cl2 removed much of the color, and the aqueous phase was made basic and reextracted with 3x100 mL CH2Cl2 (Methylene Chloride). Removal of the solvent yielded 13.0 g of a yellow-colored oil that was distilled. The fraction boiling at 80-90 °C at 0.2 mm weighed 10.2 g and was water-white. It was dissolved in 60 mL of IPA (Is 91% store bought ok), neutralization with concentrated HCl, and diluted with 120 mL of anhydrous Et2O (Is DCM ok to substitute)which produced a lasting turbidity. Crystals formed spontaneously which were removed by filtration, washed with Et2O, and air dried to provide 10.4 g of 3,4-methylenedioxyamphetamine hydrochloride (MDA) with a mp of 187-188 °C. [b]



		hypo (Hive Addict) 04-13-04 12:51 No 500562				no problem...
						if you have access to LAH and nitroethane, that is. http://www.google.com/search?q=millenium



		Sunlight (Pioneer Researcher) 04-13-04 23:43 No 500684				And piperonal
						Don't forget the aldehyde.



		amine (Hive Bee) 04-16-04 19:22 No 501107				If you can get safrole you can look into this...
						If you can get safrole you can look into this route: Safrole to Isosafrole (via Isomerization) Isosafrole to MDP2P (via Performic/Oxone/Peracetic use HCL for hydrolysis) MDP2P to the Oxime. Al/Hg reduction of the oxime. :) MDA Its all there on rhodiums MDMA page. if u need links pm me.



		lastchance (Stranger) 04-19-04 23:51 No 501685				Al/Hg reduction of the oxime. is stupid
						SWIM has done hundreds of reactions converting MDP2P tp MDA but would never consider AL/HG it is very dangerous to the environment. I spelt a little in my back yard and after 2 years nothing would grow there. Sodium Cyano is much better. My question is the first part of PIHKAL MDA complete? I am not a morone and I think it is I just wanted some one ike Rohodium to confirm it. I sure do miss Strike.



		Barium (Heavyweight Chempion(eer)) 04-20-04 09:06 No 501753				If you know what you are doing Al(Hg) is not...
						If you know what you are doing Al(Hg) is not enviromentally dangereous since the mercury is easy to recover.



		Sunlight (Pioneer Researcher) 04-20-04 23:13 No 501887				MDA by CTH reductive amination
						I believe is the best method if you can get Pd/C and ammonium formate. 70-80 % yeild using 20-30 % of 10 % catalyst, and washing it with NaOH solution extensively and then with water till pH 7 it works 5-7 times. UTFSE.

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