acetic anhydride

Discussion in 'Drug Chemistry' started by wangtangkiki, Dec 19, 2006.

  1. wangtangkiki

    wangtangkiki Member

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    how would i go about obtaining a small amount? i saw something about acetic acid condensating can form it.. but iono..
     
  2. polymer

    polymer Senior Member

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    from roguesci.org

    acetic anhydride (CH3CO)2O CAS number 108-24-7

    mp -73 bp 139 d 1.080 m 102.09 c $?.??
    Safety Data: MSDS Corrosive, Flammable

    Synonyms: acetic acid anhydride; acetic oxide; acetyl anhydride; acetyl ether; acetyl oxide; ethanoic anhydrate; ethanoic anhydride

    Synthesis: Acetic anhydride is a very handy organic compound that has fallen into ill repute thanks to the drug dealers. It is technically a watched chemical, but you will only have to answer questions at gunpoint if you buy over 250 gallons. Even so, you will most likely be put on The List if you buy any, and you will have to come up with a bunch of explanations as to what you are going to do with it. Acetic anhydride is very corrosive and must be kept away from moisture, as it will decompose into acetic acid.
    Into a 200-mL Florence flask, add 70 g of finely pulverized, anhydrous sodium acetate. Set the flask up for simple distillation, instead of a thermometer in the top of the flask use an addition funnel. Slowly add, by dropwise addition, 45.5 mL of acetyl chloride from the addition funnel. After half of the acetyl chloride has been added, stop the addition and stir the reaction mix with a glass stirring rod. Afterwards, continue the addition the rest of the way. If at any point during the addition some material should distill over, pour it back into the reaction flask and decrease the rate of addition to prevent this. After the addition is complete, remove the addition funnel, stop up the flask, and distill with flame or hot plate. The crude acetic anhydride thus obtained needs to be purified by distillation. Set up for a simple distillation, add 3 g of finely pulverized, anhydrous sodium acetate to the reaction flask, and then pour in the crude acetic anhydride. The sodium acetate will convert any remaining acetyl chloride into the anhydride. The receiving flask should be under a water shower for cooling. Place a large funnel (a cheap plastic one will work fine) under the flask with a tube leading to the sink, pour cold water over the top of the receiving flask. The receiving flask can also be held directly under the faucet in the sink. Commence the distillation; the yield should be about 50 g of pure acetic anhydride.
     
  3. KParker730

    KParker730 Member

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    hey we just used this stuff in chemistry to make aspirin!
     
  4. polymer

    polymer Senior Member

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    yep.. with salicylic acid
     
  5. KParker730

    KParker730 Member

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    yeah, what kind of drugs do you synth with it?
     
  6. polymer

    polymer Senior Member

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    acetyl salicylate is probably what you made...that's aspirin.

    acetic anhydride is good for putting an acetyl group on a primary alcohol. (i.e. acetyl-THC)
     
  7. Eeso

    Eeso Member

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    A route is ketene from the thermal decomposition of acetone vented into glacial acetic acid.

    However - this is for all intents a modified industrial process - ketene is not something to be trifled with. The toxicity is said to be somewhere on the order of phosgene.


    Be safe.
     
  8. polymer

    polymer Senior Member

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    phosgene is some nasty stuff; they kept some in the fridge of the polymer lab, as it's a free-radical initiator for polyurethanes.

    that gas was used to fill the trenches during WWI. it was so heavy, it would sink into the trenches; and if you were to inhale some, you couldn't cough it out, only bloody lung tissue. when soldiers tried to crawl out of the trenches, they'd be annihilated by the newly developed water-cooled Browning machine guns.

    but yeah...that's some high toxicity.
     
  9. Eeso

    Eeso Member

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    Supposedly it's way harder to miss than phosgene.
     

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