反应详情

To the solution of benzyl 3-(tert-butyldimethylsilyloxy)propylcarbamate obtained in step 2 (5 g, 15.5 mmol) in tetrahydrofuran (20 ml), sodium hydride (1.24 g, 31 mmol, 60% in mineral oil) and iodomethane (3.86 ml, 62 mmol) were added slowly. The reaction temperature was warmed up to room temperature, and stirred for overnight. The reaction was completed quenched by water and organic material was extracted with ether. After evaporation of volatile material under reduced pressure, the residue was purified with silica gel column chromatography (EtOAC:Hx=1:10) to give the title compound (4.9 g, 94%) as light yellow oil.

1. customThe reaction was completed quenched by water and organic material
2. extractionwas extracted with ether
3. customAfter evaporation of volatile material under reduced pressure
4. customthe residue was purified with silica gel column chromatography (EtOAC:Hx=1:10)