反应详情

温度

35 °C

A mixture of N,N-dimethyl-2,6-dichloro-3-nitrobenzenesulfonamide (2.64 g, 8.83 mmol), 60% sodium hydride (1.06 g, 26.5 mmol) and water (191 mg, 10.6 mmol) was heated to 35° C. while kept under argon atmosphere for 16 hours. The solvent was evaporated. when The reaction was almost complete as indicated by 1H NMR. The residue was diluted with ethyl acetate and washed with 1N aq. HCl. The solvent was concentrated to give the crude material. Column chromatography on silica gel, eluting with ethyl acetate/hexane/acetic acid (40/58/2, v/v/v), gave the desired product (2.3 g, 93%). EI-MS (m/z)279.5 (M−).

1. customThe solvent was evaporated
2. additionThe residue was diluted with ethyl acetate
3. washwashed with 1N aq. HCl
4. concentrationThe solvent was concentrated
5. customto give the crude material
6. washColumn chromatography on silica gel, eluting with ethyl acetate/hexane/acetic acid (40/58/2, v/v/v)