反应详情

A solution of 2-(phenylsulphenyl)-4-trifluoromethylbenzoic acid (11.5 g) and thionyl chloride (11.4 g) in dichloroethane containing a few drops of DMF was heated at reflux for 1.5 hours. The mixture was evaporated to dryness and methanol was added. The mixture was heated at reflux for 1 hour and evaporated to dryness. It was treated with water and extracted with ether, washed with sodium carbonate solution (2M), water, dried (Na2SO4) and filtered. The filtrate was evaporated to dryness and the residue was triturated with cyclohexane and filtered to give methyl 2-(phenylsulphenyl)-4-trifluoromethylbenzoate (10.5 g) as a white solid, m.p. 55°-60° C.

1. temperatureat reflux for 1.5 hours
2. customThe mixture was evaporated to dryness and methanol
3. additionwas added
4. temperatureThe mixture was heated
5. temperatureat reflux for 1 hour
6. customevaporated to dryness
7. additionIt was treated with water
8. extractionextracted with ether
9. washwashed with sodium carbonate solution (2M), water
10. dry with materialdried (Na2SO4)
11. filtrationfiltered
12. customThe filtrate was evaporated to dryness
13. customthe residue was triturated with cyclohexane
14. filtrationfiltered