HRID41281

反应详情

EQUATION

反应方程式

HRID 41281 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a toluene (0.9 mL) solution of 3-[2,6-dimethoxy-4-(methoxymethyl)phenyl]-6-methoxy-N-propylpyrazolo[5,1-b][1,3]thiazole-7-amine (70 mg, 0.179 mmol) were added 2-bromopyridine (56.6 mg, 0.358 mmol), sodium tert-butoxide (25.8 mg, 0.269 mmol) and bis(tri-tert-butylphosphine)palladium (4.57 mg, 0.009 mmol), and the mixture was stirred at 100° C. for five hours. After the reaction mixture was returned to room temperature, water was added to the reaction mixture, and the reaction mixture was extracted with ethyl acetate, and the solvent was distilled off under reduced pressure. The residue was purified by medium pressure amino silica gel column chromatography (n-heptane/ethyl acetate: 10% then 50%) to obtain the title compound (18.2 mg, 0.0388 mmol).

WORKUP

后处理

  1. customwas returned to room temperature
  2. extractionthe reaction mixture was extracted with ethyl acetate
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue was purified by medium pressure amino silica gel column chromatography (n-heptane/ethyl acetate