Skindeep_Assrash (Hive Bee)
08-19-01 08:41
No 205785
      Subbing Tert with MeOH & Pd(AcO)2 with PdCl2 ?  Bookmark   

SWISA needs to know if this recipe has anything wrong with it. READ CAREFULLY:

 To a 5L 2-neck flask equipped with condendor and addition funnel goes:
      -100gm safrol
      -5gm Palladium Chloride
      -250ml methanol
  Commence with the magnetic stirring full bore while bringing temp to 80c.

      -over 30 minutes time frame,start adding H2O2 when temp
       reaches 78-80C.
Maintain reflux at 78-82C for a TOTAL of 6 hours.

Flood with dH2O and clean up with solvent (DCM, toluene, etc)

 The original synthesis was found in TSII but used Tert-butyl alcohol instead of MeOH and Palladium acetate instead of Palladium Chloride.

 Are these modifications realistic if one wants to yield the precoius oil (smells to ketone)?

Assrash Ouch!
 
 
 
 
    terbium
(Hive Addict)
08-19-01 08:57
No 205789
      Re: Subbing Tert with MeOH & Pd(AcO)2 with PdCl2 ?  Bookmark   


The original synthesis was found in TSII but used Tert-butyl alcohol instead of MeOH and Palladium acetate instead of Palladium Chloride.

Are these modifications realistic if one wants to yield the precoius oil (smells to ketone)?



There is quite a bit of difference btween tert-butanol and methanol.

 
 
 
 
    Osmium
(Stoni's sexual toy)
08-19-01 15:34
No 205820
      Re: Subbing Tert with MeOH & Pd(AcO)2 with PdCl2 ?  Bookmark   

Besides, the tert-BuOH thing doesn't work.
 
 
 
 
    sunlight
(Hive Bee)
08-19-01 18:16
No 205845
      Re: Subbing Tert with MeOH & Pd(AcO)2 with PdCl2 ?  Bookmark   

Noone have get something interesting with it. I remember some test with methanol and didn't work.