反应 #169658

反应方程式

L-valine methylester

N-methyl morpholine

EDCI.HCl

nicotinic acid

→

required product

3-methyl-2-[pyridine-3-carbonyl]-amino-butyric acid methyl ester

溶剂

ethyl acetate

DCM

反应条件

后处理

1. 1
   洗涤washed with water (3×100mL)
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 L-valine methylester (3.0 g, 2.29 mmol), in DCM (30 mL) were added N-methyl morpholine (11.5 mL, 11.45 mmol), EDCI.HCl (8.7 g, 45.8 mmol) and nicotinic acid (3.3 g, 27.4 mmol). The mixture was allowed to stir at room temperature (25° C.) over 3 h under nitrogen atmosphere. The resulting mixture was diluted with ethyl acetate (200 mL), washed with water (3×100mL) 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 sticky solid (2.0 g, 38%).

来源