反应详情

13.8 g (0.1 mol) of dried potassium carbonate and 1.6 g (0.01 mol) of potassium iodide are suspended in a solution of 19.4 g (0.1 mol) of 4-(trifluoromethylthio)phenol in 250 ml of dry butanone and 15.4 g (0.15 mol) of 3-chloro-3-methyl-1-butyne are added dropwise. The mixture is then heated under reflux with stirring for 20 hours, 15.4 g of 3-chloro-3-methyl-1-butyne and 13.8 g of potassium carbonate are added once again and the mixture is further heated under reflux for 40 hours. Inorganic constituents are filtered off, the solution is concentrated, and the residue is taken up in 200 ml of methylene chloride and extracted using 1N NaOH solution. The organic phase is washed with water, dried and concentrated, and the residue is filtered through silica gel.

1. additionare added dropwise
2. temperatureThe mixture is then heated
3. temperatureunder reflux
4. temperaturethe mixture is further heated
5. temperatureunder reflux for 40 hours
6. filtrationInorganic constituents are filtered off
7. concentrationthe solution is concentrated
8. extractionextracted
9. washThe organic phase is washed with water
10. customdried
11. concentrationconcentrated
12. filtrationthe residue is filtered through silica gel