反应 #1880968

反应方程式

2-ethyl butanoic acid

HOBt

EDC

2(S)-pyrrolidine-carboxylic acid ethylester hydrochloride

NMM

→

desired product

收率 75.1%

N-(2-Ethylbutyryl)-2(S)-pyrrolidine-carboxylic acid ethylester

收率 75.1%

溶剂

dichloromethane

反应条件

后处理

1. 1
   workup.ADDITIONwere added
2. 2
   workup.STIRRINGstirred at room temperature for overnight
3. 3
   洗涤After then, the reaction mixture was washed with water, 1% sodium hydroxide solution
4. 4
   干燥The organic layer was dried over sodium sulfate
5. 5
   其他the solvents were removed in vacuo
6. 6
   其他Purification by silica gel chromatography

实验过程

To dichloromethane solution (350 ml) of 2-ethyl butanoic acid 5.68 g (48.9 mmol) under cooling on ice-water, HOBt 6.76 g (50 mmol), EDC 9.6 g (50 mmol) were added, stirring was continued for 30 min. 2(S)-pyrrolidine-carboxylic acid ethylester hydrochloride 8 g (45 mmol), NMM 4.55 g (45 mmol) were added to the reaction mixture and then stirred at room temperature for overnight. After then, the reaction mixture was washed with water, 1% sodium hydroxide solution, and then water sequentially. The organic layer was dried over sodium sulfate and the solvents were removed in vacuo. Purification by silica gel chromatography gave a desired product as an oil (8.16 g). NMR was consistent with the desired title product.

来源