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
CONDITIONS
反应条件
- 温度
- 27.5 °C
PROCEDURE
实验过程
Methylene dichloride (130 ml) and water (65 ml) are added to enantiomerically pure esomeprazole calcium salt (13 gm, obtained in step-II) under stirring at 25-30° C., the contents are cooled to 15° C. and then pH of the mass is adjusted to 7.0-7.5 with acetic acid. The resulting mass is stirred for 15 minutes, separated the layers and the aqueous layer is extracted with methylene dichloride (100 ml). The total organic layer is washed with 5% NaCl solution (65 ml), dried over sodium sulfate and the resulting organic layer is distilled under vacuum at 40° C. and then co-distilled with methanol (100 ml) to give 10.3 gm of enantiomerically pure esomeprazole as residue (enantiomeric purity: 100%).
WORKUP
后处理
- temperaturethe contents are cooled to 15° C.
- stirringThe resulting mass is stirred for 15 minutes
- customseparated the layers
- extractionthe aqueous layer is extracted with methylene dichloride (100 ml)
- washThe total organic layer is washed with 5% NaCl solution (65 ml)
- dry with materialdried over sodium sulfate
- distillationthe resulting organic layer is distilled under vacuum at 40° C.