HRID1957930

反应详情

EQUATION

反应方程式

HRID 1957930 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Under an atmosphere of argon, 2.50 g (19.6 mmol) of 2-methyl-5-chloropyridine and 4.38 g (23.5 mmol) of N-(tert-butyloxycarbonyl)piperazine are dissolved in 50 ml of absolute toluene. 2.26 g (23.5 mmol) of sodium tert-butoxide, 0.37 g (0.59 mmol) of BINAP and 0.36 g (0.39 mmol) of tris(dibenzylideneacetone)dipalladium are then added, and the mixture is heated at 70° C. for 12 h. After cooling, diethyl ether is added to the reaction mixture, the mixture is washed three times with saturated sodium chloride solution and dried over sodium sulphate and the solvent is removed under reduced pressure. The residue is purified by flash chromatography (cyclohexane/ethyl acetate 9:1).

WORKUP

后处理

  1. temperatureAfter cooling
  2. washthe mixture is washed three times with saturated sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. customthe solvent is removed under reduced pressure
  5. customThe residue is purified by flash chromatography (cyclohexane/ethyl acetate 9:1)