HRID1992330
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
- 80 °C
PROCEDURE
实验过程
To a solution of CuCl (1 mg, 0.01 mmol) and PdCl2(PPh3)2 (0.003 g, 0.004 mmol) in DMF (2 mL) were added 2-methyl-5-[(trimethylsilyl)ethynyl]pyrimidine (0.088 g, 0.462 mmol) and tert-butyl 4-{[(trifluoromethyl)sulfonyl]oxy}-3,6-dihydropyridine-1(2H)-carboxylate (Example 2e) (0.183 g, 0.555 mmol) at room temperature. The reaction mixture was stirred for 8 h at 80° C. After cooling, the mixture was quenched with 1N HCl and extracted with ether (3×). The combined organic layers were washed with saturated aqueous NaHCO3 solution, brine and dried. Filtration and evaporation afforded a brown oil, which was purified on HPLC to give the subtitle compound (0.062 g, 45%).
WORKUP
后处理
- temperatureAfter cooling
- customthe mixture was quenched with 1N HCl
- extractionextracted with ether (3×)
- washThe combined organic layers were washed with saturated aqueous NaHCO3 solution, brine
- customdried
- filtrationFiltration and evaporation
- customafforded a brown oil, which
- customwas purified on HPLC