HRID570121
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
- 0 °C
PROCEDURE
实验过程
Crude compound 26 (445 mg) was dissolved in THF (20 ml), MeOH (10 ml) and water (10 ml). After cooling to 0° C. 1M LiOH (2 ml) was added. After 1.5 h the hydrolysis was completed and HOAc (1 ml) was added and the solution was evaporated to appr 10 ml. Water was added and the mixture was extracted with DCM (2×30 ml). The pooled organic phase was washed with NaHCO3 (aq), water, brine and dried over MgSO4. The crude product was purified by column chromatography on silica (DCM/MeOH: 100/0-80/20) to give the title compound (201 mg, 67%).
WORKUP
后处理
- customthe solution was evaporated
- additionWater was added
- extractionthe mixture was extracted with DCM (2×30 ml)
- washThe pooled organic phase was washed with NaHCO3 (aq), water, brine
- dry with materialdried over MgSO4
- customThe crude product was purified by column chromatography on silica (DCM/MeOH: 100/0-80/20)