HRID1795469

反应详情

EQUATION

反应方程式

HRID 1795469 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customquenched with 6N HCl (1 ml)
  2. extractionextracted with AcOEt
  3. washThe organic layer was washed with H2O and brine
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customThe residue was recrystallized from a mixture of MeOH, diethyl ether and hexane