HRID365401

反应详情

EQUATION

反应方程式

HRID 365401 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.5 g of (+/-)-cis-N-[2-(3,4-dimethoxyphenyl)cyclohexyl]-4-p-toluenesulfonamidobenzamide are dissolved in 100 ml of acetonitrile and 1.0 ml of phosphorus oxychloride and the solution is stirred at 50° C. for 8 h. The reaction mixture is added to 100 ml of saturated sodium hydrogencarbonate solution and extracted with ethyl acetate. The organic phase is washed with sodium hydrogencarbonate solution and water, dried using sodium sulfate and concentrated. The residue is recrystallized from ethanol. 1.8 g (53.2% of theory) of the title compound of melting point: 122° C. (decomposition) are obtained.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic phase is washed with sodium hydrogencarbonate solution and water
  3. customdried
  4. concentrationconcentrated
  5. customThe residue is recrystallized from ethanol