HRID901939
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturecooled
- customthe mixture separated
- washThe organic phase was washed with water and brine
- filtrationfiltered through phase separation paper