反应详情

Benzyl 3-hydroxypropylcarbamate obtained in step 1 (15 g, 72 mmol) was treated with imidazole (10 g, 146.9 mmol) and TBSCl (12 g, 79.6 mmol) in DMF (10 ml) at 0° C. After warming up the resulting reaction mixture to room temperature, it was stirred for 30 minutes. The resulting solution was quenched with water (50 ml), and then extracted with diethyl ether twice (50 ml×2). After evaporation of volatile material under reduced pressure, the residue was purified with silica gel column chromatography (EtOAc:Hx=1:10) to afford the title compound (23 g, 98%) as colorless oil.

1. temperatureAfter warming up
2. customthe resulting reaction mixture to room temperature
3. customThe resulting solution was quenched with water (50 ml)
4. extractionextracted with diethyl ether twice (50 ml×2)
5. customAfter evaporation of volatile material under reduced pressure
6. customthe residue was purified with silica gel column chromatography (EtOAc:Hx=1:10)