反应详情

温度

45 °C

A mixture of 2,6-dichloro-3-nitrobenzenesulfonamide (2.61 g, 9.64 mmol), 60% sodium hydride (1.15 g, 28.9 mmol) and water (174 μL, 9.64 mmol) was heated to 45° C. while kept at argon atmosphere for 3 days. The reaction was monitored by 1H NMR. 0.1 equivalent water was added to the mixture when the reaction was not completed. The solvent was evaporated when the reaction almost completed 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 (50/48/2, v/v/v), gave the desired product (1.87 g, 77%). EI-MS (m/z)250.84, 252.89 (M−).

1. additionwas added to the mixture when the reaction
2. customThe solvent was evaporated when
3. customthe reaction
4. washwashed with 1N aq. HCl
5. concentrationThe solvent was concentrated
6. customto give the crude material
7. washColumn chromatography on silica gel, eluting with ethyl acetate/hexane/acetic acid (50/48/2, v/v/v)