HRID532501

反应详情

EQUATION

反应方程式

HRID 532501 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

2.00 g (17.8 mmol) of furan-2-carboxylic acid were suspended in 25 mL of toluene and one drop of dimethylformamide was added to the mixture. 1.95 ml of thionylchloride (26.8 mmol) were added at room temperature and the reaction mixture was stirred at 80° C. for two hours. After removal of the solvent, toluene was added and the evaporation was repeated. The obtained residue was then dissolved in 5 ml of dichloromethane and the solution was added dropwise to a solution containing 1.70 g of pyridazin-4-yl-amine (17.8 mmol) and 2.73 ml of triethyl amine (19.6 mmol) in 20 ml of dichloromethane. The mixture was stirred at room temperature for 2 days and washed twice with water. The organic layer was dried over Na2SO4, filtered and the solvent was removed under vacuum to give the title compound as a brown solid (1.9 g, 54%, 95% purity).

WORKUP

后处理

  1. customAfter removal of the solvent, toluene
  2. additionwas added
  3. customthe evaporation
  4. dissolutionThe obtained residue was then dissolved in 5 ml of dichloromethane
  5. additionthe solution was added dropwise to a solution
  6. stirringThe mixture was stirred at room temperature for 2 days
  7. washwashed twice with water
  8. dry with materialThe organic layer was dried over Na2SO4
  9. filtrationfiltered
  10. customthe solvent was removed under vacuum