反应详情

20 g (91.6 mmol) of 2,5-difluorobenzophenone 1 (Fluka) was dissolved in 400 ml of DMSO. 7.0 g (150 mmol) of lithium sulfide (Fluka) was added under argon. After three hours at 120° C., the mixture was allowed to cool to room temperature. It was shaken with 200 ml of 2 M HCl aq. and 500 ml of ethyl acetate. The organic phase was washed twice with NaCl solution, dried over MgSO4, filtered, and concentrated. 24 g of crude product 2 was obtained as a reddish oil. TLC (n-heptanelethyl acetate 3:1) gave Rf=0.3 (starting material 1 Rf=0.4). C13H9FOS (232.28). MS (M+H)+=233.1.

1. washThe organic phase was washed twice with NaCl solution
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. custom24 g of crude product 2 was obtained as a reddish oil