HRID2417665
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The requisite 2-(4-amino-1,3-dimethyl-5-pyrazolyl)-3,3-dimethylimidazoline is prepared as follows. p-Toluenesulfonic acid (10 g, 0.055 mol) is added to 5 g (0.057 mol) of 1,2-diamino-2-methylpropane and to the resulting hot (100°) melt is added 7 g (0.05 mol) of 4-amino-5-cyano-1,3-dimethylpyrazole. The mixture is heated in an oil bath at 185°-195° C. for six hours. The residue, an amorphous yellow solid is dissolved in 250 ml of chloroform and stirred with 40 ml of conc. ammonium hydroxide. The organic layer is separated, dried (MgSO4), and evaporated in vacuo to give 9 g (90%) of slightly crude title compound as a viscous purple oil.
WORKUP
后处理
- temperatureThe mixture is heated in an oil bath at 185°-195° C. for six hours
- customThe organic layer is separated
- dry with materialdried (MgSO4)
- customevaporated in vacuo