HRID1992330

反应详情

EQUATION

反应方程式

HRID 1992330 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureAfter cooling
  2. customthe mixture was quenched with 1N HCl
  3. extractionextracted with ether (3×)
  4. washThe combined organic layers were washed with saturated aqueous NaHCO3 solution, brine
  5. customdried
  6. filtrationFiltration and evaporation
  7. customafforded a brown oil, which
  8. customwas purified on HPLC