HRID2035545

反应详情

EQUATION

反应方程式

HRID 2035545 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

25 mg of 4-benzylamino-6-chloropyridine-3-carboxyamide (the compound of Example 1) was dissolved in 0.5 ml of toluene, to which 13.5 mg of 4-aminopyridine, 2 mg of palladium (II) acetate, 248 mg of potassium carbonate and 11 mg of 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl were added, and stirred at 100° C. for 28 hours. After cooling, the insoluble substances were filtered off, the filtered product was washed with toluene, combined with the filtrate, and the solvent was evaporated. The residue obtained was purified by silica gel column chromatography (chloroform:methanol=10:1) to obtain 4.8 mg (yield 16%) of the title compound as a slight yellow crystalline powder.

WORKUP

后处理

  1. additionwere added
  2. temperatureAfter cooling
  3. filtrationthe insoluble substances were filtered off
  4. washthe filtered product was washed with toluene
  5. customthe solvent was evaporated
  6. customThe residue obtained
  7. customwas purified by silica gel column chromatography (chloroform:methanol=10:1)