反应 #169679

反应方程式

niacin

N-methyl morpholine

L-leucinemethyl ester hydrochloride

→

required product

收率 72.6%

4-methyl-2-[pyridine-3-carbonyl]-amino-pentanoic acid methyl ester

收率 72.6%

溶剂

DCM

DCM

反应条件

后处理

1. 1
   洗涤washed with water (3×100 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 (1.35 g, 11.0 mmol) in DCM (20 mL) were added N-methyl morpholine (3.34 g, 33.00 mmol) EDCI.HCl (4.2 g, 22.02 mmol), and L-leucinemethyl ester hydrochloride (2.0 g, 11.0 mmol). The mixture was allowed to stir at room temperature (25° C.) over 2.5 h under nitrogen atmosphere. The resulting mixture was diluted with DCM (200 mL), washed with water (3×100 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 white solid (2.0 g, 72%).

来源