HRID1957930
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 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
- temperatureAfter cooling
- washthe mixture is washed three times with saturated sodium chloride solution
- dry with materialdried over sodium sulphate
- customthe solvent is removed under reduced pressure
- customThe residue is purified by flash chromatography (cyclohexane/ethyl acetate 9:1)