HRID1253405

反应详情

EQUATION

反应方程式

HRID 1253405 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of N-[2,6-dibromo-4-(1,2,2,3,3,3-hexafluoro-1-trifluoromethylpropyl)-phenyl]-3-nitro-4-(1,2,4-triazol-1-yl)benzamide (Example I2) (675 mg, 0.98 mmol) in a mixture of ethanol and water (20 ml and 4 ml, respectively) was added aqueous hydrochloric acid (37% w/v) (0.25 ml) and iron metal powder (5550 mg, 9.8 mmol). The reaction mixture was stirred at 80° C. for 1 hour. The mixture was filtered through a silica gel pad and the filtrate concentrated. The residue was purified by column chromatography on silica gel (eluent: cyclohexane/ethyl acetate 1:1) to give Compound No. B4 of Table B (372 mg, 58% yield).

WORKUP

后处理

  1. filtrationThe mixture was filtered through a silica gel pad
  2. concentrationthe filtrate concentrated
  3. customThe residue was purified by column chromatography on silica gel (eluent: cyclohexane/ethyl acetate 1:1)
  4. customto give Compound No