反応 #169658

反応方程式

L-valine methylester

N-methyl morpholine

EDCI.HCl

nicotinic acid

→

required product

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

溶媒

ethyl acetate

DCM

反応条件

後処理

1. 1
   洗浄washed with water (3×100mL)
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 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%).

出典