The Vespiary

The Hive => Methods Discourse => Topic started by: Skindeep_Assrash on August 19, 2001, 08:41:00 AM

Title: Subbing Tert with MeOH & Pd(AcO)2 with PdCl2 ?
Post by: Skindeep_Assrash on August 19, 2001, 08:41:00 AM: 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!
Title: Re: Subbing Tert with MeOH & Pd(AcO)2 with PdCl2 ?
Post by: terbium on August 19, 2001, 08:57:00 AM: 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.
Title: Re: Subbing Tert with MeOH & Pd(AcO)2 with PdCl2 ?
Post by: Osmium on August 19, 2001, 03:34:00 PM: Besides, the tert-BuOH thing doesn't work.
Title: Re: Subbing Tert with MeOH & Pd(AcO)2 with PdCl2 ?
Post by: sunlight on August 19, 2001, 06:16:00 PM: Noone have get something interesting with it. I remember some test with methanol and didn't work.