反应 #169664

反应方程式

niacin

N-methyl morpholine

EDCI.HCl

L-glutamic acid dimethyl ester

→

required product

收率 97.2%

2-benzoyl amino-pentane dioic acid dimethyl ester

收率 97.2%

溶剂

DCM

DCM

反应条件

后处理

1. 1
   洗涤washed with water (3×50 mL)
2. 2
   干燥dried over sodium sulphate
3. 3
   其他The crude product obtained upon evaporation of the solvent
4. 4
   其他was further purified by silica gel column chromatography

实验过程

To a solution of niacin (1.4 g, 11.42 mmol) in DCM (20 mL) were added N-methyl morpholine (3.76 mL, 34.2 mmol), EDCI.HCl (4.36 g, 34.2 mmol) and L-glutamic acid dimethyl ester (2.0 g, 11.42 mmol). The mixture was allowed to stir at room temperature (25° C.) over 3 h under nitrogen atmosphere. The resulting mixture was diluted with DCM (100 mL), washed with water (3×50 mL) and dried over sodium sulphate. The crude product obtained upon evaporation of the solvent was further purified by silica gel column chromatography to obtain required product as pale yellow oil (3.1 g, 73%).

来源