HRID2373531

反应详情

EQUATION

反应方程式

HRID 2373531 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

The residue obtained in Example 2A was transferred to a 2 L 4-necked round bottom flask and 500 ml of 2N aqueous HCl was added at a temperature ranging from about 25° C. to about 30° C. The reaction mass was heated to a temperature ranging from about 80° C. to about 85° C. and maintained for between 4 to 5 hours. After completion of the reaction (detected by HPLC/TLC), the reaction mass was cooled to a temperature ranging from about 50° C., and 500 ml of toluene was charged to the reaction mass and maintained for 30 minutes at a temperature of about 50° C. The reaction mass was further stirred at a temperature ranging from about 25° C. to about 30° C. for about 30 minutes. The solids were filtered, separated, and then washed twice with 100 ml of toluene. The product was dried to get crude oxcarbazepine of 97-98% purity as determined by HPLC.

WORKUP

后处理

  1. customranging from about 25° C. to about 30° C
  2. temperatureThe reaction mass was heated to a temperature
  3. customranging from about 80° C. to about 85° C.
  4. temperaturemaintained for between 4 to 5 hours
  5. customAfter completion of the reaction (detected by HPLC/TLC)
  6. temperaturethe reaction mass was cooled to a temperature
  7. customranging from about 50° C.
  8. filtrationThe solids were filtered
  9. customseparated
  10. washwashed twice with 100 ml of toluene
  11. customThe product was dried