HRID1886948

反应详情

EQUATION

反应方程式

HRID 1886948 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of potassium hexacyanoferrate(III) (670 mg, 2.04 mmol) in water (5 mL) at 90° C. was added dropwise over 5 minutes a solution of 4-chloro-N-(4-(methylthio)phenyl)benzothioamide (150 mg, 0.51 mmol) in ethanol (2 mL) and 3M aqueous sodium hydroxide solution (1.4 mL, 4.08 mmol). The resulting mixture was heated at 90° C. for 30 minutes. After cooling, the precipitate formed was filtered off and washed with water to give a yellow solid. The yellow solid was purified by column chromatography eluting using a gradient (hexanes to ethyl acetate/hexanes 5:95 v/v) to afford 100 mg (67%) of the title compound (LCMS RT=9.37 min, MH+ 292.2)

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe precipitate formed
  3. filtrationwas filtered off
  4. washwashed with water
  5. customto give a yellow solid
  6. customThe yellow solid was purified by column chromatography
  7. washeluting