反应详情

1,3-Dimethyl-5-pyrazolamine (3.33 g; 0.030 mol) is dissolved in ethanol (35 ml) and methyl-2-(3-nitrobenzyliden)acetoacetate (6.75 g; 0.27 mol) is added thereto. The mixture is refluxed for about 5 hours, then the solvent is evaporated under reduced pressure and the residue is taken up in methylene chloride, washed with 2% hydrochloric acid and then with saturated aqueous sodium bicarbonate, the organic phase is dried over sodium sulphate and then the solvent is evaporated. The solid compound of the title is recovered by filtration, after taking up in ethyl ether. M.p. 163°-166° C.

1. temperatureThe mixture is refluxed for about 5 hours
2. customthe solvent is evaporated under reduced pressure
3. washwashed with 2% hydrochloric acid
4. dry with materialwith saturated aqueous sodium bicarbonate, the organic phase is dried over sodium sulphate
5. customthe solvent is evaporated
6. filtrationThe solid compound of the title is recovered by filtration