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             Synthesis of MDP2P from isosafrole with peracetic acid
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     Semtex Enigma: Peracetic ala Rhodium's suggestion, Scaled exactly 5X:


Chemicals:

* Peracid:
- 1650ml of Glacial Acetic Acid
- 325ml of 30% H2O2
- 5ml of H2SO4
- Olefin:
- 500ml Acetone
- 325g of Isosafrole
- Solvents:
- 7500ml of Water
- 1500ml of DCM
- 600ml of MeOH
- H2SO4(15%):
- 525g(285ml) of Concentrated H2SO4
- 3215ml of Water

* Wash(s):
- 1250ml of Water
- 1250ml of NaOH 5% solution

* Drying:
- 50g of Anhydrous MgSO4

* Distillation:
- 100ml of Cooking oil to prevent scorching

Procedure:

- Mix the peracetic acid chemicals together in an appropreate sized flask(3L+),
  swirl or stir solution until thouroughly mixed and let stand for 12 hours.

- Combine the olefin chemicals and place into the freezer to chill.

- Bring the peracid solution down to 5C with the help of an ice/salt/water bath.
  While magnetically stirring this solution sitting in the ice bath, add the now
  chilled olefin solution to the peracid solution at such a rate that the
  mixture stays below 40C. After all of the olefin has been added, let the
  solution stir for 16 hours, letting the ice bath melt away and the solution
  come to room temperature on it's own.

- After the 16 hours of stirring has elapsed, flood solution, or pour solution
  into 7500ml cold water and mix thouroughly. After which time one extracts this
  mixture with 3 X 500ml DCM. The extractions are combined and the solvent
  removed via distillation to yeild a thick, dark red syrup.

- This syrup is taken up with 600ml MeOH and added to the 3500ml H2SO4 solution
  and lightly refluxed for two hours. After which the flask is cooled under
  running water and/or the use of an ice bath, do not proceed until solution has
  reached room temperature or lower.

- Using a large sepratory funnel or by simply pouring off the acid layer collect
  the dark bottom layer BEFORE extracting this mixture 3 X 400ml DCM(you did
  reuse the DCM from the first extraction, didn't you?). Combine the extracts
  with the dark layer which was first collected and proceed.

- Wash this dark mixture of ketone/solvent with 1250ml of water, then with the
  1250ml of the 5% NaOH solution which was made previously. Please note that the
  seperation with the second wash will be difficult to see, therefor the use of
  a light is favorable to determine the different layers(similar to the first
  seperation of a Benzoquinone wacker wash).

- Dry organic phase over/thru 50g of anhydrous MgSO4(made by baking epsom salts
  at 300C for a couple of hours, let cool, then grinding into a powder) making
  sure to filter off the MgSO4, and washing the filter cake with a small amount
  of DCM. The solvent is removed and kept for a later run, the resulting residue
  is Combined with 100ml of vegitable cooking oil and distilled under vac to
  yeild ketone(>200g).

Oh yeah, I forgot, some amounts were changed with out a change in yeild. I think
SWIM said that the amount of GAA could be reduced to 1500ml and the resulting
glycol can be taken up in 500ml of MeOH and refluxed with 2500ml of H2SO4(15%)
(thanks Strikey, baby!!!), instead of the above amounts.

At any rate, keep us posted, I'm sure your "dreams" will work out VERY positive,
cept for that list I chem, GAA... BTW, if anyone gets credit for this, I think
it should be Rhodium. As he proposed this almost a year ago, and Gyro gave SWIM
a kick in the ass to get on it when he/she reported success with it. This is NOT
a new method, just seems to be one which got lost in the shuffle somehow. Have
fun and please remember that the peracetic is explosive, so please try to treat
it with some respect (caution)...

The whole thread on this can be found at:

http://hive.lycaeum.org/ubb_board/Forum5/HTML/000581.html

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