反应详情

温度

0 °C

29.0 g of N-acetyl-4-(2,3-dichlorophenyl)-3-trifluoromethylpyrrole are dissolved in 500 ml of diethyl ether. This solution is subsequently cooled to 0° C., and to it are added portionwise 13.7 g of lithium aluminium hydride. The mixture is afterwards stirred for 1 hour, and there are then added dropwise at 5° C. 55 ml of 4% sodium hydroxide solution, in the course of which elementary hydrogen is given off, and the mixture is subsequently stirred for a further hour at room temperature. The mixture is then filtered; the filtrate is dried over magnesium sulfate, again filtered, and concentrated by evaporation. The resulting oil is distilled at 150°/8×10-5 mbar. By covering it with hexane, there is obtained from the distillate 3-trifluoromethyl-4-(2,3-dichlorophenyl)pyrrole in the form of colourless crystals, m.p. 63°-65° C.

1. additionthere are then added dropwise at 5° C
2. stirringthe mixture is subsequently stirred for a further hour at room temperature
3. filtrationThe mixture is then filtered
4. dry with materialthe filtrate is dried over magnesium sulfate
5. filtrationagain filtered
6. concentrationconcentrated by evaporation
7. distillationThe resulting oil is distilled at 150°/8×10-5 mbar