反应详情

Add triethylamine (3.73 mL, 26.7 mmol) to a solution of piperidin-3-yl-trityl-amine (7.63 g, 22.3 mmol) in dichloromethane (125 mL), follow by dropwise addition of methyl chloroformate (1.76 mL, 22.7 mmol). Stir the reaction at room temperature under nitrogen overnight. Wash the reaction is wash with saturated aqueous sodium bicarbonate solution, brine, dry over magnesium sulfate and concentrate. Purify by flash chromatography on silica gel (eluting with 0–20% ethyl acetate/hexane) to give 6.51 g of the title compound as a white solid, 73% yield. 1H NMR: consistent with structure.

1. customthe reaction at room temperature under nitrogen overnight
2. washWash the reaction
3. washis wash with saturated aqueous sodium bicarbonate solution, brine
4. dry with materialdry over magnesium sulfate
5. concentrationconcentrate
6. customPurify by flash chromatography on silica gel (eluting with 0–20% ethyl acetate/hexane)