反应详情

温度

105 °C

Aluminium chloride (267 g) was added in portions over 30 minutes to a stirred solution of 4-ethylphenol (122.1 g.) and 4-chlorobenzoyl chloride (140 ml.) in dry 1,1,2,2-tetrachloroethane (800 ml.). The mixture was heated at 105° C. for 22 hours with stirring, and on cooling a mixture of ice (600 g) and concentrated hydrochloric acid was added slowly. A vigorous reaction occurred and some material was lost. The remaining material was separated, the aqueous fraction extracted twice with chloroform (200 ml.), and the combined organic layers evaporated to a dark oil which was distilled in vacuo giving two main fractions: B (17.4 g) 150°-160° C. at 0.3 mmHg; C (110.8 g) 160°-168° C. at 0.3 mmHg. The title compound was crystallised by cooling to -20° C. and recrystallised from n-hexane at 0° C. to give a yellow crystalline solid m.p. 35°-8° C.

1. temperatureon cooling
2. additionwas added slowly
3. customA vigorous reaction
4. customThe remaining material was separated
5. extractionthe aqueous fraction extracted twice with chloroform (200 ml.)
6. customthe combined organic layers evaporated to a dark oil which
7. distillationwas distilled in vacuo
8. customgiving two main fractions
9. customB (17.4 g) 150°-160° C.
10. customC (110.8 g) 160°-168° C.
11. customThe title compound was crystallised
12. temperatureby cooling to -20° C.
13. customrecrystallised from n-hexane at 0° C.