反应详情

(1R,2R)-2-[[trans-2-[(1E,3E)-4-(4-Cyano-2-fluorophenyl)-1,3-butadienyl]-1,3-dioxan-5-yl]thio]-1-(2,4-difluorophenyl)-1-[(1H-1,2,4-triazol-1-yl)methyl]propyl 4-(allyloxycarbonyloxy)butyrate (352 mg, 4.94×10−4 mol) obtained from Example 11-(3) and bis(triphenylphosphine)dichloropalladium (2 mg) were dissolved in dichloromethane (3 ml). Tributyltin hydride (215 mg, 7.39×10−4 mol) was slowly added to the mixture at room temperature over a period of 5 minutes. After stirring at room temperature for 15 minutes further, hexane was added to the reaction mixture. The insoluble liberated oily material was separated by removing the supernatant liquid slowly. The insoluble residue was further washed twice with hexane. The oily residue was subjected to chromatography on a silica gel (15 g) column (eluent; ethyl acetate:hexane=3:1˜1:0) to afford the title compound (289 mg, 93% yield) as a colorless amorphous solid.

1. customThe insoluble liberated oily material was separated
2. customby removing the supernatant liquid slowly
3. washThe insoluble residue was further washed twice with hexane