反应详情

Sodium hydrosulfite (10.2 g, 58.7 mmol) dissolved in water (66 ml) was added dropwise to a vigorously stirred solution of 3-chloro-5-[(2-fluoro-3-methyl-6-nitrophenyl)oxy]benzonitrile (3.0 g, 9.78 mmol) dissolved in THF (33 mL). The reaction was stirred for 1 h then EtOAc (100 mL) was added and the layers were separated. The aqueous layer was extracted with EtOAc (2×50 mL). The organic extracts were combined, dried over Na2SO4, filtered and evaporated to afford the title compound (2.5 g, 92%) as a solid. 1H NMR (400 MHz, DMSO-d6): δ ppm 7.68 (d, 1H), 7.26 (dd, 1H), 7.16 (t, 1H), 6.85 (t, 1H), 6.51 (dd, 1H), 5.17 (d, 2H), 2.06 (d, 3H) MS: m/z 277.2 (M+1).

1. customthe layers were separated
2. extractionThe aqueous layer was extracted with EtOAc (2×50 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customevaporated