HRID2074075

反应详情

EQUATION

反应方程式

HRID 2074075 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 argon atmosphere, 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 a saturated sodium chloride solution and dried over sodium sulfate and the solvent is removed in vacuo. 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 a saturated sodium chloride solution
  3. dry with materialdried over sodium sulfate
  4. customthe solvent is removed in vacuo
  5. customThe residue is purified by flash chromatography (cyclohexane/ethyl acetate 9:1)