HRID1797389

反应详情

EQUATION

反应方程式

HRID 1797389 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sumatriptan (10.0 grams), water (50.0 ml), succinic acid (3.99 grams) and acetonitrile (100.0 ml) were heated to reflux temperature. The reaction mass was stirred for 15–30 minutes at reflux and filtered in hot condition. The solvent was distilled off completely from the filtrate under reduced pressure at a temperature of below 35–45° C. Cyclohexane (100 ml) was added to the resulting residual mass and stirred for 1–2 hours at a temperature of 25–35° C. to crystallize the solid. Then the solid was filtered, washed with cyclohexane (50 ml) and on subsequent drying under vacuum at a temperature of 25–35° C. there resulted the amorphous form of Sumatriptan succinate of the invention.

WORKUP

后处理

  1. temperatureto reflux temperature
  2. temperatureat reflux
  3. filtrationfiltered in hot condition
  4. distillationThe solvent was distilled off completely from the filtrate under reduced pressure at a temperature of below 35–45° C
  5. additionCyclohexane (100 ml) was added to the resulting residual mass
  6. stirringstirred for 1–2 hours at a temperature of 25–35° C.
  7. customto crystallize the solid
  8. filtrationThen the solid was filtered
  9. washwashed with cyclohexane (50 ml)
  10. customon subsequent drying under vacuum at a temperature of 25–35° C.