HRID526678

反应详情

EQUATION

反应方程式

HRID 526678 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of eslicarbazepine (18 gm), triethylamine (8.5 gm), dimethylaminopyridine (0.1 gm), acetic anhydride (8.7 gm) and dichloromethane (90 mL) was stirred at about 20-25° C. for about 4 hrs. To the resulting solution water was added and resulting solution was stirred for about 15 minutes. Organic layer was separated and washed with 1 N HCl solution followed by washing with water. The solvent was distilled out completely. Ethyl acetate was added to the resulting residue followed by stirring at about 25-30° C. for about 3 hrs. The resulting solid was filtered, washed and dried to obtain the title compound (Yield: 80%; HPLC purity: 99.8%; Chiral purity: 99.3%; d0.9 50.7 μm, d0.5 17.3 μm, d0.1 6.0 μm).

WORKUP

后处理

  1. customresulting solution
  2. customOrganic layer was separated
  3. washwashed with 1 N HCl solution
  4. washby washing with water
  5. distillationThe solvent was distilled out completely
  6. additionEthyl acetate was added to the resulting residue
  7. stirringby stirring at about 25-30° C. for about 3 hrs
  8. filtrationThe resulting solid was filtered
  9. washwashed
  10. customdried