HRID1713498

反应详情

EQUATION

反应方程式

HRID 1713498 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionthe residue was diluted with ethyl acetate
  3. washThe reaction solution was washed with water and saturated brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationThe solid was filtered off
  6. concentrationthe filtrate was concentrated
  7. customThe residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:1)
  8. concentrationconcentrated
  9. washThe residue was washed with hexane
  10. filtrationcollected by filtration