HRID2089002

反应详情

EQUATION

反应方程式

HRID 2089002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a solution of Example 7a (5.72 g, 15 mmol) in 60 mL ethanol/water (5/1) was added powdered KOH (2 g, 35 mmol). The resulting solution was heated at 40° C. for 2 hours. Most of the solvent was removed in vacuo, and the residue was diluted with ethyl acetate. A solid was filtered from the material and discarded. The organics were washed with water, brine, dried over MgSO4, filtered, and concentrated. The crude material was triturated with dichloromethane and filtered, giving 3.5 g of the title compound as a white solid. MS (ESI+) m/z 263.6 (M+H)+.

WORKUP

后处理

  1. customMost of the solvent was removed in vacuo
  2. additionthe residue was diluted with ethyl acetate
  3. filtrationA solid was filtered from the material
  4. washThe organics were washed with water, brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude material was triturated with dichloromethane
  9. filtrationfiltered