反应 #2504844

ord-a6e93a42d1764eadad75bcf770abc096

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度is heated in an oil bath at 180°-200° C. for seven hours
  2. 2
    其他The organic layer is separated
  3. 3
    干燥dried over MgSO4
  4. 4
    其他evaporated in vacuo

实验过程

A mixture of 7 g (0.05 mol) of 4-amino-5-cyano-1,3-dimethylpyrazole, 5 g (0.057 mol) of 2,3-diaminobutane and 10.5 g (0.055 mol) of p-toluene sulfonic acid hydrate is heated in an oil bath at 180°-200° C. for seven hours. The yellow melt is dissolved in 200 ml of chloroform and stirred with 100 ml of 20% aqueous sodium carbonate solution. The organic layer is separated, dried over MgSO4 and evaporated in vacuo to give 9.5 g of 2-(4-amino-1,3-dimethyl-5-pyrazolyl)-4,5-dimethylimidazoline and characterized as a dihydrochloride salt, mp 250° C. from 20% isopropanolic HCl and ethyl acetate.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04469868uspto-grants-1984_09