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
- 0 °C
PROCEDURE
实验过程
To a solution of cyclopropylamine (1.0 g, 18 mmol) and triethylamine (3.7 mL, 27 mmol) in tetrahydrofuran (20 mL) was added 2-nitrobenzenesulfonyl chloride (3.9 g, 18 mmol) at 0° C., and the mixture was stirred at 0° C. for 1 hour. The solvent was distilled off under reduced pressure, and the residue was diluted with ethyl acetate. The reaction solution was washed with water and saturated brine and dried over magnesium sulfate. The solid was filtered off, and the filtrate was concentrated. The residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:1) and concentrated. The residue was washed with hexane and collected by filtration to obtain the title compound (3.7 g, 87%).
WORKUP
后处理
- distillationThe solvent was distilled off under reduced pressure
- additionthe residue was diluted with ethyl acetate
- washThe reaction solution was washed with water and saturated brine
- dry with materialdried over magnesium sulfate
- filtrationThe solid was filtered off
- concentrationthe filtrate was concentrated
- customThe residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:1)
- concentrationconcentrated
- washThe residue was washed with hexane
- filtrationcollected by filtration