HRID891459

反应详情

EQUATION

反应方程式

HRID 891459 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

N-Bromosuccinimide (1.76 g, 9.89 mmol) and potassium thiocyanate (1.75 g, 18.0 mmol) in methanol (30 ml) were stirred for 15 minutes at room temperature. The reaction mixture was cooled to 0° C., and 3-fluoroaniline (1.00 g, 9.0 mmol) was added dropwise. The mixture was stirred at 0° C. for 2 h. Solvent was removed under vacuum, and the residue was washed with dichloromethane. The mixture was filtered to remove succinimide by-product, and the solution was washed with water, brine, and dried (MgSO4). Solvent was removed under vacuum to afford the desired product as a colorless oil. Yield 1.45 g (96%). 1H NMR.

WORKUP

后处理

  1. customSolvent was removed under vacuum
  2. washthe residue was washed with dichloromethane
  3. filtrationThe mixture was filtered
  4. customto remove succinimide by-product
  5. washthe solution was washed with water, brine
  6. dry with materialdried (MgSO4)
  7. customSolvent was removed under vacuum