HRID901939

反应详情

EQUATION

反应方程式

HRID 901939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Glycine methyl ester hydrochloride (2.2 g, 18 mmol), diisopropylethylamine (2.9 g, 29 mmol), 18-crown-6 (370 mg, 1.4 mmol) and potassium fluoride (1.6 g, 28 mmol) were added to a solution of 1-fluoro-2-nitrobenzene (2 g, 14 mmol) in acetonitrile (150 ml). The mixture was heated at 80° C. for 48 h and cooled. 0.3N potassium hydrogen sulphate and ethyl acetate were added and the mixture separated. The organic phase was washed with water and brine, filtered through phase separation paper and reduced. Chromatography (15% EtOAc/85% 6080 petroleum ether) afforded N-(2-nitrophenyl)glycine methyl ester as a yellow solid (2.5 g, 85%).

WORKUP

后处理

  1. temperaturecooled
  2. customthe mixture separated
  3. washThe organic phase was washed with water and brine
  4. filtrationfiltered through phase separation paper