HRID2407711

反应详情

EQUATION

反应方程式

HRID 2407711 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The compound prepared in Example 127 (0.65 g) was suspended in tetrahydrofuran (20 mL) and then lithium aluminum hydride solution (1 M; 4.44 mL) was added dropwise to the solution at room temperature and stirred overnight. The reaction mixture was transferred dropwise to a stirred room temperature saturated aqueous solution of Rochelle's salt (sodium potassium tartrate). The mixture was diluted with ethyl acetate and the biphasic mixture stirred rapidly for 30 minutes. The layers were separated and the organics washed with brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure to afford the crude material (0.53 g), which was used without further purification possessing the following physical data.

WORKUP

后处理

  1. customwas transferred dropwise to a stirred room temperature
  2. stirringthe biphasic mixture stirred rapidly for 30 minutes
  3. customThe layers were separated
  4. washthe organics washed with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure