HRID1759790

反应详情

EQUATION

反应方程式

HRID 1759790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

67 mg of Na2WO4, 8 drops of acetic acid and 19 mL of H2O were placed in a flask and the mixture was heated to 65° C. 19 mL (153 mmol) of 4-methylthioaniline was added followed by 34.5 mL (337 mmol) of H2O2 dropwise. The mixture was stirred at 65° C. for 1.5 h and, after cooling, 800 mL of 1N HCl and 500 mL of CHCl3 was added. The layers were separated and the aqueous phase was washed with more CHCl3. The aqueous phase was basified with 25% NaOH and extracted with CHCl3. The organic phase was washed with brine and dried over MgSO4. The solvent was removed, yielding the product as a white solid (19.80 g, 75%).

WORKUP

后处理

  1. temperatureafter cooling
  2. customThe layers were separated
  3. washthe aqueous phase was washed with more CHCl3
  4. extractionextracted with CHCl3
  5. washThe organic phase was washed with brine
  6. dry with materialdried over MgSO4
  7. customThe solvent was removed