Modern MDA. How do you make MDA from helional?

kaydoe

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I found two methods but they are written i just can't understand it.
 

kaydoe

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, High Yield MDAEasy, High Yield MDAExerpt from something I heard somewhere.......The Finkelstein reaction is the word for the day! Bromosafrole in acetone treated with KI to form the iodide (iodine is a much better leaving group). Iodosafrole forms the amine with NH3 alone at normal pressure. Start to finish MDA in the +90%! Or, as per twodogs:

Quote:The following reactions make use of a commercially available product that goes under various trade names eg Helional, Floramelon.

The aldoxime of this aldehyde undergoes the Beckman rearrangement with Nickel Acetate to give the amide that is then easily transformed to the amine by the Hoffman reaction.

The Hoffman reaction can be achieved with 4.2% NaOCl sold in supermarkets as bleach.I don't have any references as this was done a while ago.

The aldoxime and Hoffman reactions are pretty standard.

The Beckman rearrangement of this particular product using Nickel Acetate is my own work.It doesn't get any easier that this.

The aldoxime.

100 grms of the aldehyde is placed in 200 mls of ETOH with 50-60 grms of Hydroxylamine Hydrochloride * in 100 mls of H2O. 40 grms of Sodium Carbonate in 100 mlsof H2O is slowly added with stirring.
Once addition is complete the mixture is stirred overnight then filtered to give about 100 grms of the aldoxime. If the aldoxime doesn't solidify add more hydroxylamine and base.

The amide.

100 grms of the aldoxime is mixed with 300 mls of xylene and 2 grms of Nickel Acetate ** is added and refluxed for 5 hours. About 100 mls of xylene is distilledoff and the mixture is left to cool. About 70 grms of the amide separates and is filtered and dried,. Can be recrystallized with xylene.

The amine.

To a solution of 10 grms NaOH in 200 mls H2O in a 500 mls flask is added 20 grmsof the amide and 250 grms of 4.2 % NaOCl . The mixture is then heated to 80C with stirring. At about 50 to 60C the mixture can become white as the carbonate forms. At 70-80C an oil separates. (This is crude MDA). The solution was cooled and extracted with xylene. The solution was filtered and the filtrate washed with xylene and the xylene portions added together. About 100 mls of conc HCL was added to the xylene shaken and separated. The aqueous solution was extracted with xylene and the xylene separated. The amine was then liberated from the aqueous portion with NaOH and worked up in the usual way to give MDA

• *Hydroxylamine: HCL200 mls nitromethane, 300 mls Acetic acid and 300 mls HCL are heated to just below reflux and held there for 2 hours then refluxed for 12 hours. The solution isreduced to half gone the cooled in fridge overnight and filtered.

• **Nickel Acetate: 20 grms of nickel oxide (black) is dissolved in Acetic acid and heated with stirring until the mixture turns pale green. The excess Acetic is drained off , the rest is dried and powdered.Making Hydroxylamine HCl http://psychonaut.com/post-35899.html?f=43
 

HIT MONKEY

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, High Yield MDAEasy, High Yield MDAExerpt from something I heard somewhere.......The Finkelstein reaction is the word for the day! Bromosafrole in acetone treated with KI to form the iodide (iodine is a much better leaving group). Iodosafrole forms the amine with NH3 alone at normal pressure. Start to finish MDA in the +90%! Or, as per twodogs:

Quote:The following reactions make use of a commercially available product that goes under various trade names eg Helional, Floramelon.

The aldoxime of this aldehyde undergoes the Beckman rearrangement with Nickel Acetate to give the amide that is then easily transformed to the amine by the Hoffman reaction.

The Hoffman reaction can be achieved with 4.2% NaOCl sold in supermarkets as bleach.I don't have any references as this was done a while ago.

The aldoxime and Hoffman reactions are pretty standard.

The Beckman rearrangement of this particular product using Nickel Acetate is my own work.It doesn't get any easier that this.

The aldoxime.

100 grms of the aldehyde is placed in 200 mls of ETOH with 50-60 grms of Hydroxylamine Hydrochloride * in 100 mls of H2O. 40 grms of Sodium Carbonate in 100 mlsof H2O is slowly added with stirring.
Once addition is complete the mixture is stirred overnight then filtered to give about 100 grms of the aldoxime. If the aldoxime doesn't solidify add more hydroxylamine and base.

The amide.

100 grms of the aldoxime is mixed with 300 mls of xylene and 2 grms of Nickel Acetate ** is added and refluxed for 5 hours. About 100 mls of xylene is distilledoff and the mixture is left to cool. About 70 grms of the amide separates and is filtered and dried,. Can be recrystallized with xylene.

The amine.

To a solution of 10 grms NaOH in 200 mls H2O in a 500 mls flask is added 20 grmsof the amide and 250 grms of 4.2 % NaOCl . The mixture is then heated to 80C with stirring. At about 50 to 60C the mixture can become white as the carbonate forms. At 70-80C an oil separates. (This is crude MDA). The solution was cooled and extracted with xylene. The solution was filtered and the filtrate washed with xylene and the xylene portions added together. About 100 mls of conc HCL was added to the xylene shaken and separated. The aqueous solution was extracted with xylene and the xylene separated. The amine was then liberated from the aqueous portion with NaOH and worked up in the usual way to give MDA

• *Hydroxylamine: HCL200 mls nitromethane, 300 mls Acetic acid and 300 mls HCL are heated to just below reflux and held there for 2 hours then refluxed for 12 hours. The solution isreduced to half gone the cooled in fridge overnight and filtered.

• **Nickel Acetate: 20 grms of nickel oxide (black) is dissolved in Acetic acid and heated with stirring until the mixture turns pale green. The excess Acetic is drained off , the rest is dried and powdered.Making Hydroxylamine HCl http://psychonaut.com/post-35899.html?f=43
kaydoeYes it works. I'm having trouble with separating the salt from the mda in the end? I don't understand the same thing as work up as usual? Can someone explain? I tested what I do have, black and smokes instantly.
 

archae

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Well, if you have an easy to follow protocol what is the problem? What EXACTLY don't you understand in the procedure?
 

kaydoe

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Well, if you have an easy to follow protocol what is the problem? What EXACTLY don't you understand in the procedure?
archaeTHIS
"The solution was cooled and extracted with xylene. The solution was filtered and the filtrate washed with xylene and the xylene portions added together. About 100 mls of conc HCL was added to the xylene shaken and separated. The aqueous solution was extracted with xylene and the xylene separated. The amine was then liberated from the aqueous portion with NaOH and worked up in the usual way to give MDA"

its written poorly.
 
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archae

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THIS
"The solution was cooled and extracted with xylene. The solution was filtered and the filtrate washed with xylene and the xylene portions added together. About 100 mls of conc HCL was added to the xylene shaken and separated. The aqueous solution was extracted with xylene and the xylene separated. The amine was then liberated from the aqueous portion with NaOH and worked up in the usual way to give MDA"

its written poorly.
kaydoeIt lacks a bit in clarity, but nothing insurmountable if you understand what's going on
Here you use xylene to extract your amine (produced from the amide) that is "floating" in the reaction mixture. As the amine is in the freebase form, it's insoluble in water but soluble in organic solvants.

Then you acidify with HCl to convert the freebase to the hydrochloride salt which become insoluble in xylene and goes into the water. You wash the amine-containing water with xylene to remove any non-water soluble impurities, and finally you rebasify the water to yield the freebase, your final product.
 

twok

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It lacks a bit in clarity, but nothing insurmountable if you understand what's going on
Here you use xylene to extract your amine (produced from the amide) that is "floating" in the reaction mixture. As the amine is in the freebase form, it's insoluble in water but soluble in organic solvants.

Then you acidify with HCl to convert the freebase to the hydrochloride salt which become insoluble in xylene and goes into the water. You wash the amine-containing water with xylene to remove any non-water soluble impurities, and finally you rebasify the water to yield the freebase, your final product.
archaeALDEHYDE WOULD MDP2P?, I HAVE MDP2P BUT I DON'T UNDERSTAND IF IT GOES INTO THIS SYNTHESIS AND IN WHAT PART
 

HIT MONKEY

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THIS
"The solution was cooled and extracted with xylene. The solution was filtered and the filtrate washed with xylene and the xylene portions added together. About 100 mls of conc HCL was added to the xylene shaken and separated. The aqueous solution was extracted with xylene and the xylene separated. The amine was then liberated from the aqueous portion with NaOH and worked up in the usual way to give MDA"

its written poorly.
kaydoeHello friends, I have a question=
MDA hydrochloride floats in water. How can I make it crystallize?
 

UWe9o12jkied91d

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Piperonal ---(henry reaction with EtNO2)---> metielene dioxy phenylpropene -----NaBH4, AlHg etc-----------> Amine
 

Macondor

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Raxd

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And whats forms if use nitromethane instade of nitroethane in the herny reaction
MacondorIf you use MeNO2 (nitroMETHANE) and not EtNO2 ( nitroETHANE) for your Henry Reaction you will get a nitrostyrene , in this case 3,4 metylenedioxy-beta-nitrostyrene . This looks a lot like what you want to get , also yellowish crystals but will not produce an active amine !
If you use EtNO2 you will get your desired substrate (3,4 metylendioxyphenyl2-nitropropene) that will reduce to an active amine ( MDA ) .
 

kaydoe

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rebasify ? so add more Naoh?
 

kaydoe

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I think i get it. i will post pictures and the whole process.
 

archae

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yes, you bring the pH back up using a base, NaOH is adequate for this
 

HIT MONKEY

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Hello friends, I am a newbie and have no knowledge about chemistry.
I would like to know what crystallization method you used in the final step.
 

kamikaze3030

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I am achieving 60% yield in the synthesis of MDA Helional + Hydroxylamine. The best way for large-scale production.
 

HIT MONKEY

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Hello friends. I have a question
1. In the final step, you use the crystallization method with a stream of HCl gas. Is that right or does it burn?

2. Amide.

100 g aldoxime is mixed with 300 mL xylene and 2 g nickel acetate, added and refluxed for 5 hours. Distill approximately 100 mL xylene and allow the mixture to cool. Amide approximately 70. The grams are separated and filtered and dried. Can be recrystallized with xylene.
=How much heat can you give?
3. Aldoxime.
If aldoxime does not harden Add more hydroxylamine and base.
How much hydroxylamine and base should I add?

thank you
 
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kamikaze3030

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Hello friends. I have a question
1. In the final step, you use the crystallization method with a stream of HCl gas. Is that right or does it burn?

2. Amide.

100 g aldoxime is mixed with 300 mL xylene and 2 g nickel acetate, added and refluxed for 5 hours. Distill approximately 100 mL xylene and allow the mixture to cool. Amide approximately 70. The grams are separated and filtered and dried. Can be recrystallized with xylene.
=How much heat can you give?
3. Aldoxime.
If aldoxime does not harden Add more hydroxylamine and base.
How much hydroxylamine and base should I add?

thank you
HIT MONKEYI don't do it that way, friend. I'm doing it differently, totally different.
 
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HIT MONKEY

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Yes, I succeed. It is the best method to do it on a large scale. Simple and efficient. Few easily accessible equipment and supplies.
kamikaze3030Hello friend, I have a question.
In the last step you just use
(NaOH) in case it crystallizes, right?
And the .PH value should be 7.5, right?
I don't know much about chemistry.
If I'm going to confess, it's that I don't know. After adding the substance (NaOH), what must be done to get MDA? I want to ask you Can you tell me?
 

kamikaze3030

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Hello friend, I have a question.
In the last step you just use
(NaOH) in case it crystallizes, right?
And the .PH value should be 7.5, right?
I don't know much about chemistry.
If I'm going to confess, it's that I don't know. After adding the substance (NaOH), what must be done to get MDA? I want to ask you Can you tell me?
HIT MONKEYMy method is different from yours. I don't do it that way.
 
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