反应详情

温度

65 °C

To a stirred solution of 4-nitrobenzyl bromide (10.0 g, 46.3 mmol) in DMF (25 mL) was added sodium methanesulfinate (7.1 g, 69.4 mmol). The reaction mixture was stirred at 65° C. for 30 minutes, and then partitioned between water (30 mL) and EtOAc (30 mL). The organic fraction was separated, washed with water (2×30 ml), dried (Na2SO4), filtered and concentrated in vacuo to give the title compound (7.5 g, 75%) as a yellow solid that was used without further purification. δH (DMSO-d6) 8.28 (2H, d, J 8.8 Hz), 7.70 (2H, d, J 8.8 Hz), 4.72 (2H, s), 2.97 (3H, s).

1. custompartitioned between water (30 mL) and EtOAc (30 mL)
2. customThe organic fraction was separated
3. washwashed with water (2×30 ml)
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo