反応 #169664

反応方程式

niacin

N-methyl morpholine

EDCI.HCl

L-glutamic acid dimethyl ester

→

required product

収率 97.2%

2-benzoyl amino-pentane dioic acid dimethyl ester

収率 97.2%

溶媒

DCM

DCM

反応条件

後処理

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

実験手順

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%).

出典