HRID526682

反应详情

EQUATION

反应方程式

HRID 526682 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
37.5 °C

PROCEDURE

实验过程

A solution of eslicarbazepine (15.0 gm), pyridine (8 mL), dimethylaminopyridine (0.17 gm) in dichloromethane (150 mL) was cooled to 5-10° C. Added acetyl chloride (7.6 mL) at about 5-10° C. followed by stirring at 35-40° C. for about 5-6 h. Washed the reaction mass with 0.5N HCl solution (45 mL) and followed by washing the organic layer with water (100 mL). Distilled out the solvent completely under vacuum to obtain crude eslicarbazepine acetate. The residue was dissolved in a mixture (60 mL) of dichloromethane and ethyl acetate (1:1) at 35-40° C. then cooled to 25-30° C. Reaction mass was filtered, washed with ethyl acetate and dried to obtain the title compound (m. p. 186.0-187.2° C.).

WORKUP

后处理

  1. customat about 5-10° C.
  2. washWashed the reaction mass with 0.5N HCl solution (45 mL)
  3. washby washing the organic layer with water (100 mL)
  4. distillationDistilled out the solvent completely under vacuum
  5. customto obtain crude eslicarbazepine acetate
  6. temperaturethen cooled to 25-30° C
  7. customReaction mass
  8. filtrationwas filtered
  9. washwashed with ethyl acetate
  10. customdried