反应详情

To 5.6 g. of potassium hydroxide of the grade described above was added 25 ml. of butanol, and the mixture was stirred for 15 minutes. To it was added dropwise 2.8 g. of 1,1,1-trichloro-2-(3-trifluoromethylphenyl)ethane, and the mixture was stirred under reflux for 3.75 hours. It was then cooled to 5°, and to it was added dropwise 6 ml. of concentrated sulfuric acid. The mixture was then stirred under reflux for 30 minutes and cooled overnight. It was then reheated to reflux, and about 22 ml. of butanol and water was distilled away. The mixture was then cooled again, and diluted with about 50 ml. of water. The aqueous layer was separated and extracted with three 25 ml. portions of dichloromethane. The organic layers were combined, washed with 1 N sodium hydroxide, dried over sodium sulfate and evaporated under vacuum to obtain 3.0 g. of impure product. The product was dissolved in 30 ml. of dichloromethane, washed with water, dried over sodium sulfate and concentrated under vacuum again to obtain 2.67 g. of product, found to be 83% pure by vapor phase chromatography.

1. additionabove was added 25 ml
2. additionTo it was added dropwise 2.8 g
3. temperatureunder reflux for 3.75 hours
4. temperatureIt was then cooled to 5°
5. additionto it was added dropwise 6 ml
6. temperatureunder reflux for 30 minutes
7. temperaturecooled overnight
8. temperatureto reflux
9. distillationof butanol and water was distilled away
10. temperatureThe mixture was then cooled again
11. additiondiluted with about 50 ml
12. customThe aqueous layer was separated
13. extractionextracted with three 25 ml
14. washwashed with 1 N sodium hydroxide
15. dry with materialdried over sodium sulfate
16. customevaporated under vacuum
17. customto obtain 3.0 g
18. dissolutionThe product was dissolved in 30 ml
19. washof dichloromethane, washed with water
20. dry with materialdried over sodium sulfate
21. concentrationconcentrated under vacuum again
22. customto obtain 2.67 g