HRID1167611

反应详情

EQUATION

反应方程式

HRID 1167611 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

The compound obtained in Step D (400 mg; 2.42 mmol) is suspended in 10 ml of water. Potassium carbonate (10 eq.; 24.2 mmol; 3.35 g), tetrabutylammonium bromide (0.05 eq.; 0.12 mmol; 40 mg) and bromoacetonitrile (8 eq.; 19.37 mmol; 1.35 ml) are then added. The mixture is stirred vigorously for 12 hours at 70° C. After returning to ambient temperature, the product formed is extracted with dichloromethane. The organic phase is dried over MgSO4, filtered, and then concentrated under reduced pressure. The residue obained is purified by flash chromatography on silica gel (eluant: PE/AcOEt (1/1)). The title product is obtained in the form of a solid.

WORKUP

后处理

  1. customAfter returning to ambient temperature
  2. customthe product formed
  3. extractionis extracted with dichloromethane
  4. dry with materialThe organic phase is dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue obained is purified by flash chromatography on silica gel (eluant: PE/AcOEt (1/1))