反应详情

温度

65 °C

Triton B (5.85 ml) was added dropwise to 4-chlorophenylacetone (21.8 grams) in 78 ml of tert.butanol. Next crotononitrile (9.17 grams) was likewise added with initial cooling to lower the temperature to about 20° C. Since the reaction was not exothermic, no additional cooling was necessary after the desired temperature was reached. The reaction was then heated to 65° C. for 21/2 hours and, after chilling in an ice bath, 262 ml of 1N HCl was added in portions. Next the reaction mixture was extracted with ether, washed with water, dried, and evaporated in vacuo. An oil resulted which was distilled under vacuum, yield 18.6 grams, b.p. 130°-131° C.

1. temperaturewith initial cooling
2. customto about 20° C
3. temperatureno additional cooling
4. temperatureafter chilling in an ice bath
5. extractionNext the reaction mixture was extracted with ether
6. washwashed with water
7. customdried
8. customevaporated in vacuo
9. customAn oil resulted which
10. distillationwas distilled under vacuum, yield 18.6 grams, b.p. 130°-131° C.