HRID1797389
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto reflux temperature
- temperatureat reflux
- filtrationfiltered in hot condition
- distillationThe solvent was distilled off completely from the filtrate under reduced pressure at a temperature of below 35–45° C
- additionCyclohexane (100 ml) was added to the resulting residual mass
- stirringstirred for 1–2 hours at a temperature of 25–35° C.
- customto crystallize the solid
- filtrationThen the solid was filtered
- washwashed with cyclohexane (50 ml)
- customon subsequent drying under vacuum at a temperature of 25–35° C.