HRID268609
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
3-(Trifluoromethyl)phenyl isocyanate (0.093 g, 0.50 mmole) was slowly added to a solution of 2a (0.12 g, 0.42 mmole) in dichloromethane (20 mL) at 0° C. The solution was allowed to warm to room temperature and stirred for 18 h. The reaction was then quenched with water (20 mL), and the organic layer was dried over anhydrous sodium sulfate, filtered and concentrated. The organic residue was purified by flash chromatographey on silica gel, eluting with dichloromethane/2.0 M ammonia in ethyl alcohol (96:4) to give 3a (0.045 g, 34%) as a white solid; MS (EI)=476 (M+).
WORKUP
后处理
- customThe reaction was then quenched with water (20 mL)
- dry with materialthe organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe organic residue was purified by flash chromatographey on silica gel
- washeluting with dichloromethane/2.0 M ammonia in ethyl alcohol (96:4)