反应详情

To a flame-dried flask was added 8.1 g. of sodium methoxide, 125 ml. of toluene and 21 ml. of methanol. The mixture was brought to reflux at 85°-87°, and to it was added dropwise a mixture of 22.8 g. of methyl (3-trifluoromethylphenyl)acetate and 12.9 g. of phenylacetonitrile. The apparatus was then set up for distillation, and the mixture was heated to 110°, removing about 46 ml. of distillate. The mixture was then cooled to about 12°, and to it was added 50 ml. of ice-water. The aqueous layer was removed and washed with 20 ml. of cold toluene. The organics were combined and washed with cold water. The aqueous layers were combined, and the pH was adjusted to 3.5 with cold hydrochloric acid. The oily product was collected by extracting the aqueous portion with three 40 ml. portions of dichloromethane, drying the organic layer over sodium sulfate and evaporating it under vacuum to obtain 30.5 g. of oil, which was 89% pure product by vapor phase chromatography.

1. additionTo a flame-dried flask was added 8.1 g
2. temperatureto reflux at 85°-87°
3. additionto it was added dropwise
4. additiona mixture of 22.8 g
5. distillationThe apparatus was then set up for distillation
6. temperaturethe mixture was heated to 110°
7. customremoving about 46 ml
8. temperatureThe mixture was then cooled to about 12°
9. additionto it was added 50 ml
10. customThe aqueous layer was removed
11. washwashed with 20 ml
12. washwashed with cold water
13. customThe oily product was collected
14. extractionby extracting the aqueous portion with three 40 ml
15. dry with materialportions of dichloromethane, drying the organic layer over sodium sulfate
16. customevaporating it under vacuum
17. customto obtain 30.5 g