HRID1666606

反应详情

EQUATION

反应方程式

HRID 1666606 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a solution of 2 M cyclohexylmagnesium bromide in diethyl ether (3.3 mL) was added a solution of 0.5 M zinc chloride in THF (14 mL) under nitrogen atmosphere, and the mixture was stirred at room temperature for 20 min. N-methylpyrrolidine (10 mL) was added, the mixture was stirred for 5 min, followed by addition of Pd(PtBu3)2 (0.13 g) and 2,4-dichloroquinoline (1.0 g), and the mixture was stirred at room temperature for 4 h. Water was added to the reaction mixture, and the mixture was extracted with chloroform. The organic layer was dried with anhydrous sodium sulfate, the desiccant was removed by filtration, the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate=6:1) to obtain 2-chloro-4-cyclohexylquinazoline (1.1 g).

WORKUP

后处理

  1. stirringthe mixture was stirred for 5 min
  2. stirringthe mixture was stirred at room temperature for 4 h
  3. extractionthe mixture was extracted with chloroform
  4. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  5. customthe desiccant was removed by filtration
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate=6:1)