反应详情

Imidazole (3.00 g, 44.0 mmol) and tert-butyldimethylsilyl chloride (6.63 g, 44.0 mmol) were added to 1-(benzyloxycarbonyl)piperidin-3-yl methanol (9.15 g, 36.7 mmol) in N,N-dimethylformamide (40 mL). The solution was stirred at room temperature for 6 hours. Subsequently, water was added and the mixture was extracted with ethyl acetate. The extract washed with brine and was dried over magnesium sulfate, followed by evaporation of the solvent. Purification of the residue by silica gel column chromatography (hexane:ethyl acetate=20:1->5:1) gave 13.2 g (99%) of the desired compound as a colorless oil.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe extract washed with brine
3. dry with materialwas dried over magnesium sulfate
4. customfollowed by evaporation of the solvent
5. customPurification of the residue by silica gel column chromatography (hexane:ethyl acetate=20:1->5:1)