HRID1173259
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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% o). LCMS: 224.4 (M+H)+.
WORKUP
后处理
- additionpoured over ice
- extractionextracted with EtOAc (100 mL)
- washThe organic phase was washed with H2O (2×25 mL) and saline solution (25 mL)
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo