反应详情

Tert-butyl[(3-iodobenzyl)oxy]dimethylsilane (WO9513095) (1.44 g) in dry 1-methyl-2-pyrrolidone (15 ml) and triethylamine (4 ml) was stirred at room temperature under nitrogen. 1-1′Bis(diphenylphosphino)ferrocene (110 mg) and tris(dibenzylideneacetone)dipalladium(0) (258 mg) were added and the mixture was stirred for 15 min. Cyclopentyl mercaptan (0.42 g) was then added, and the reaction mixture stirred at 60° C. for 2 h. The reaction mixture was cooled to room temperature, poured onto water and extracted with diethyl ether. The combined organic extracts were dried (MgSO4) and the solvent evaporated in vacuo. The residue was purified on a 50 g SPE, eluting with a stepped gradient of 10 to 100% dichloromethane-cyclohexane to give the title compound (1.09 g) LCMS RT=4.67 min.

1. stirringthe reaction mixture stirred at 60° C. for 2 h
2. additionpoured onto water
3. extractionextracted with diethyl ether
4. dry with materialThe combined organic extracts were dried (MgSO4)
5. customthe solvent evaporated in vacuo
6. customThe residue was purified on a 50 g SPE
7. washeluting with a stepped gradient of 10 to 100% dichloromethane-cyclohexane