反应详情

温度

175 °C

A mixture of 3-amino-pyrazole (0.06 mol), diethyl (2,4,6-trifluorophenyl)-malonate (0.06 mol, obtained from Example 1) and tributylamine (30 ml) was heated with reflux at 175° C. for four hours. The reaction mixture was cooled to 100° C. Aqueous sodium hydroxide (10.3 g/120 ml H2O) was added and the reaction mixture was stirred for 30 min. and cooled to ambient temperature. The organic Phase was separated off and the aqueous Phase was extracted with diethylether. The aqueous Phase was acidified with concentrated hydrochloric acid. The precipitate was collected by filtration and dried to yield 15.7 g (93 %) of the pale yellow product having a melting point of 280° C.

1. temperaturewas heated
2. temperatureThe reaction mixture was cooled to 100° C
3. temperaturecooled to ambient temperature
4. customThe organic Phase was separated off
5. extractionthe aqueous Phase was extracted with diethylether
6. filtrationThe precipitate was collected by filtration
7. customdried