反应详情

温度

60 °C

To a stirred, slightly warmed solution of 1.4 grams (0.003 mole) of ethyl 2-chloro-3-[4-cyano-1-(2,3,4-trichlorophenyl)-1H-pyrazol-5-yl]propionate in 25 mL of N,N-dimethylformamide was added in one portion 0.1 gram (0.004 mole) of sodium hydride. Upon completion of the addition the reaction mixture was warmed to about 60° C., where it was stirred for 1.75 hours. The reaction mixture was then allowed to cool to ambient temperature, where it was stirred for about 18 hours. The reaction mixture was again warmed to about 60° C., where it was stirred for two hours. The reaction mixture was cooled and concentrated under reduced pressure. The residue remaining was stirred with water for about 40 minutes, giving a solid that was collected by filtration. The solid was recrystallized from ethanol and water, yielding 0.6 gram of ethyl 3-[4-cyano-1-(2,3,4-trichlorophenyl)-1H-pyrazol-5-yl]acrylate, m.p. 131°-134° C. The nmr spectrum was consistent with the proposed structure.

1. additionUpon completion of the addition the reaction mixture
2. temperatureto cool to ambient temperature
3. stirringwhere it was stirred for about 18 hours
4. temperatureThe reaction mixture was again warmed to about 60° C.
5. stirringwhere it was stirred for two hours
6. temperatureThe reaction mixture was cooled
7. concentrationconcentrated under reduced pressure
8. stirringThe residue remaining was stirred with water for about 40 minutes
9. customgiving a solid
10. filtrationthat was collected by filtration
11. customThe solid was recrystallized from ethanol and water