HRID548874

反应详情

EQUATION

反应方程式

HRID 548874 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of (6-iodo-pyridazine-3-yl)-(5-methyl-3-phenyl-isoxazol-4ylmethyl)-amine (1.0 g, 2.6 mmol) in methanol (3 mL) was added sodium carbonate (270 mg, 2.6 mmol), 1,1′-bis(diphenylphosphino)ferrocene (141 mg, 0.26 mmol) and palladium(II) acetate (57 mg, 0.26 mmol). The resulting mixture was heated at 50° C. for 16 h under a carbon monoxide atmosphere. After cooling to room temperature it was filtered through Celite® and concentrated. Purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 20:80) afforded the title compound (720 mg, 87%) as a light brown solid. MS: m/e=325.3 [M+H]+.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature it
  2. filtrationwas filtered through Celite®
  3. concentrationconcentrated
  4. customPurification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 20:80)