反応 #340255

反応方程式

Clopidogrel

sulfuric acid

→

clopidogrel hydrogen sulfate

収率 105.2%

溶媒

acetone

water

反応条件

後処理

1. 1
   workup.DISTILLATIONdistilled at 50-55° C. under reduced pressure (5-10 mm)
2. 2
   workup.ADDITIONDichloromethane (100 ml) was added
3. 3
   workup.DISTILLATIONdistilled
4. 4
   その他was removed under reduced pressure (5-10 mm)

実験手順

To a solution of Clopidogrel free base (10 g, 0.031 moles) in acetone (65 ml) and water (13 ml), was added dropwise sulfuric acid (3.0 g, 0.33 mole) at 25-30° C. The solution was stirred for 15 minutes, distilled at 50-55° C. under reduced pressure (5-10 mm). Dichloromethane (100 ml) was added and distilled, the operation was repeated twice using dichloromethane (100 ml). Finally traces of water was removed under reduced pressure (5-10 mm) to give amorphous clopidogrel hydrogen sulfate (13.7 g). The amorphous form was similarly characterized by XRD, DSC, IR, chemical purity (HPLC)>99% and chiral purity (chiral HPLC) 99.8% (e.e.), % water 1.95, m.p. 110-120° C. (softens).

出典