反应详情

温度

90 °C

N-(2′,3′,5′,6′-tetrafluorophenyl)-4-ethylanilin (2.05 g) and chloro acetylchloride (1.99 g) is mixed without solvent and heated with stirring to 90° C. under nitrogen for 20 h. Tetrahydrofurane (10 ml) and aqueous sodium bicarbonate are added after cooling and stirring is continued for about 1 hour. The organic phase is diluted with toluene and washed with water three times and dried over magnesium sulfate. Evaporation and chromatography of the residue (silica, toluene) gave N-(2′,3′,5′,6′-tetrafluorophenyl)-N-chloroacetyl-4-ethylaniline (1.84 g) as a solid which is recrystallised from heptane, mp.: 72° C.

1. temperatureheated
2. temperatureafter cooling
3. stirringstirring
4. waitis continued for about 1 hour
5. washwashed with water three times
6. dry with materialdried over magnesium sulfate
7. customEvaporation and chromatography of the residue (silica, toluene)