HRID2074075
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling
- washthe mixture is washed three times with a saturated sodium chloride solution
- dry with materialdried over sodium sulfate
- customthe solvent is removed in vacuo
- customThe residue is purified by flash chromatography (cyclohexane/ethyl acetate 9:1)