HRID1958465

反应详情

EQUATION

反应方程式

HRID 1958465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 6-bromo-8-phenyl-[1,2,4]triazolo[4,3-a]pyridine (26.1 mg, 0.095 mmol), (Z)-tributyl(2-ethoxyvinyl)stannane (34.6 mg, 0.095 mmol) and tetraethylammonium chloride (16 mg, 0.095 mmol) in DMF (0.5 mL) was added PdCl2(PPh3)2 (2 mg, 0.005 mmol). The reaction was heated at 80° C. overnight, cooled to rt, added an aqueous of KF (1.1 eq) in water (95 μL) and further stirred for 30 mins, then diluted with ethyl acetate (2 mL), filtered and rinsed with ethyl acetate (8 mL). The mixture was then washed with water (2×2 mL), separated, dried and concentrated. The residue was purified by a flash column using a gradient of ethyl acetate in hexane (50-75%) as an eluent to give compound (13 mg, 52% yield).

WORKUP

后处理

  1. temperaturecooled to rt
  2. filtrationfiltered
  3. washrinsed with ethyl acetate (8 mL)
  4. washThe mixture was then washed with water (2×2 mL)
  5. customseparated
  6. customdried
  7. concentrationconcentrated
  8. customThe residue was purified by a flash column