反応 #169662

反応方程式

nicotinic acid

N-methylmorpholine

EDCI.HCl

isoleucine methyl ester

→

product

収率 72.0%

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

収率 72.0%

溶媒

DCM

DCM

反応条件

後処理

1. 1
   洗浄washed with water (3×100 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 nicotinic acid (2.0 g, 16.5 mmol) in DCM (20 mL), was added N-methylmorpholine (6.9 mL, 49.5 mmol), EDCI.HCl (6.3 g, 33.0 mmol) and isoleucine methyl ester (3.0 g, 16.5 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 product as yellow solid (2.9 g, 72%).

出典