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    Helional To MDA

    Uploaded by

    Karen Prescott
    The document provides instructions for producing MDA in 3 steps: 1. The aldoxime of commercially available aldehyde undergoes Beckman rearrangement with nickel acetate to form an amide. 2. The amide is then transformed into the amine MDA using the Hoffman reaction with a 4.2% sodium hypochlorite bleach solution. 3. The crude MDA product is extracted with xylene and purified through acid/base extraction to yield the final MDA product in a high yield of over 90%.

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    © All Rights Reserved
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    Helional To MDA

    Uploaded by

    Karen Prescott
    2K views2 pages
    The document provides instructions for producing MDA in 3 steps: 1. The aldoxime of commercially available aldehyde undergoes Beckman rearrangement with nickel acetate to form an amide. 2. The amide is then transformed into the amine MDA using the Hoffman reaction with a 4.2% sodium hypochlorite bleach solution. 3. The crude MDA product is extracted with xylene and purified through acid/base extraction to yield the final MDA product in a high yield of over 90%.

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    Mda

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    Helional to MDA

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    The document provides instructions for producing MDA in 3 steps: 1. The aldoxime of commercially available aldehyde undergoes Beckman rearrangement with nickel acetate to form an amide. 2. The amide is then transformed into the amine MDA using the Hoffman reaction with a 4.2% sodium hypochlorite bleach solution. 3. The crude MDA product is extracted with xylene and purified through acid/base extraction to yield the final MDA product in a high yield of over 90%.

    Copyright:

    © All Rights Reserved
    Download as DOC, PDF, TXT or read online from Scribd
    Download as doc, pdf, or txt
    2K views2 pages

    Helional To MDA

    Uploaded by

    Karen Prescott
    The document provides instructions for producing MDA in 3 steps: 1. The aldoxime of commercially available aldehyde undergoes Beckman rearrangement with nickel acetate to form an amide. 2. The amide is then transformed into the amine MDA using the Hoffman reaction with a 4.2% sodium hypochlorite bleach solution. 3. The crude MDA product is extracted with xylene and purified through acid/base extraction to yield the final MDA product in a high yield of over 90%.

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    © All Rights Reserved
    Download as DOC, PDF, TXT or read online from Scribd
    Download as doc, pdf, or txt
    of 2

     

    Wed, Mar. 10th, 2010, 02:27

    amEasy, 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

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