HRID2242400
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 5 °C
PROCEDURE
实验过程
To a solution of the compound of Example 1 (207 mg) in THF/H2O (8 ml/2 ml) was added LiOH (30 mg) at 5° C. The mixture was stirred at 5° C. for 20 hours, quenched with 6N HCl (1 ml) and extracted with AcOEt. The organic layer was washed with H2O and brine, dried (MgSO4) and evaporated. The residue was recrystallized from a mixture of MeOH, diethyl ether and hexane to yield the title compound (147 mg). The compound of Example 2 (301 mg) was also hydrolyzed in a similar manner to give the title compound (238 mg) mp. 196-198° C.; IR (Nujol) 3300, 3270, 1705, 1651, 1462, 1126 cm−1; MS (ESI−Q1MS) m/z 530 (M−H).
WORKUP
后处理
- customquenched with 6N HCl (1 ml)
- extractionextracted with AcOEt
- washThe organic layer was washed with H2O and brine
- dry with materialdried (MgSO4)
- customevaporated
- customThe residue was recrystallized from a mixture of MeOH, diethyl ether and hexane