反应详情

A mixture of 2-phenylsulphenyl-4-trifluoromethylbenzoic acid (11.5 g), thionyl chloride (1 1.4 g), dimethylformamide (0.2 ml) and dichloroethane was heated at reflux for 90 minutes. The solution was then concentrated under reduced pressure and the residue was dissolved in methanol and heated at reflux for one hour. The resulting solution was poured into aqueous sodium bicarbonate and extracted with ether. The organic phase was dried over anhydrous sodium sulphate, filtered and evaporated. The resulting material was crystallised from hexane to give methyl 2-phenylsulphenyl-4-trifluoromethylbenzoate (10.5 g) as white crystals, m.p. 58° C.

1. temperaturewas heated
2. temperatureat reflux for 90 minutes
3. concentrationThe solution was then concentrated under reduced pressure
4. dissolutionthe residue was dissolved in methanol
5. temperatureheated
6. temperatureat reflux for one hour
7. additionThe resulting solution was poured into aqueous sodium bicarbonate
8. extractionextracted with ether
9. dry with materialThe organic phase was dried over anhydrous sodium sulphate
10. filtrationfiltered
11. customevaporated
12. customThe resulting material was crystallised from hexane