HRID1025762

反应详情

EQUATION

反应方程式

HRID 1025762 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

To a dried flask containing 3-(trifluoromethyl)benzaldehyde oxime (1.89 g, 10 mol) in methylene chloride (100 mL) was added N-chlorosuccinimide (1.40 g, 10.5 mmol) slowly at 0° C. The reaction mixture was warmed to 45° C. for 2 h, poured over ice, diluted with H2O (20 mL), and extracted with EtOAc (100 mL). The organic phase was washed with H2O (2×25 mL) and saline solution (25 mL), dried over sodium sulfate, concentrated in vacuo to give N-hydroxy-3-(trifluoromethyl)benzenecarboximidoyl chloride (2 g, 90%). LCMS: 224.4 (M+H)+.

WORKUP

后处理

  1. additionpoured over ice
  2. extractionextracted with EtOAc (100 mL)
  3. washThe organic phase was washed with H2O (2×25 mL) and saline solution (25 mL)
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo