反应详情

To stirred phenyl-methanethiol (14.8 g, 119.36 mmol) in 175 ml DMF was added Cs2CO3 (38.89 g, 119.36 mmol) under argon. After 10 min. 1-bromo-2-chloro-3-fluoro-benzene (25 g, 119.36 mmol) in 25 ml DMF was added and stirring was continued overnight at RT and then 3 h at 80° C. After cooling the mixture was diluted with ethyl acetate/water and washed subsequently with 1 N HCl and brine. The organic layer was dried with MgSO4, filtered and evaporated. Purification by chromatography on silica gel yielded 22 g (59%) as an amorphous, colorless solid.

1. waitwas continued overnight at RT
2. custom3 h
3. customat 80° C
4. temperatureAfter cooling the mixture
5. washwashed subsequently with 1 N HCl and brine
6. dry with materialThe organic layer was dried with MgSO4
7. filtrationfiltered
8. customevaporated
9. customPurification by chromatography on silica gel
10. customyielded 22 g (59%) as an amorphous, colorless solid