反应 #355791

反应方程式

3-(Trifluoromethyl)phenyl isocyanate

2a

2-(S)-Amino-N-(1-benzyl-pyrrolidin-3-(R)-yl)-3,3-dimethyl-butyramide

→

3a

收率 34.0%

N-(1-Benzyl-pyrrolidin-3-(R)-yl)-3,3-dimethyl-2-(S)-[3-(3-trifluoromethyl-phenyl)-ureido]-butyramide

收率 34.0%

溶剂

dichloromethane

反应条件

后处理

1. 1
   其他The reaction was then quenched with water (20 mL)
2. 2
   干燥the organic layer was dried over anhydrous sodium sulfate
3. 3
   过滤filtered
4. 4
   浓缩concentrated
5. 5
   其他The organic residue was purified by flash chromatographey on silica gel
6. 6
   洗涤eluting with dichloromethane/2.0 M ammonia in ethyl alcohol (96:4)

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+).

来源