反应详情

Sodium hydride (4.87 g, 122.0 mmol, 60% dispersion in oil) was added to a solution of 2-methylimidazole (10 g, 122.0 mmol) in DMF (100 ml) and stirred at room temperature for 0.25 h. 1-Fluoro-4-nitrobenzene (17.18 g, 122.0 mmol) was added to the reaction mixture and stirred at room temperature for 16 h. Water (150 ml) and ethyl acetate (250 ml) were added, the aqueous separated and extracted with ethyl acetate (3×150 ml). The combined extracts were washed with water (3×150 ml), dried (Na2SO4) and evaporated to give the desired product (11.5 g, 47%); δ (360 MHz, CDCl3) 2.24 (3H, s, Me); 7.06 (1H, d, J=1.5 Hz, Ar-H); 7.10 (1H, d, J=1.5 Hz, Ar-H); 7.50 (2H, d, J=9.5 Hz, Ar-H); 8.38 (2H, d, J=9.5 Hz, Ar-H).

1. stirringstirred at room temperature for 16 h
2. customthe aqueous separated
3. extractionextracted with ethyl acetate (3×150 ml)
4. washThe combined extracts were washed with water (3×150 ml)
5. dry with materialdried (Na2SO4)
6. customevaporated