反应详情

To a cold (0 C) suspension of 2-amino-5-bromo-3-pyridinesulfonyl chloride (92.1 mmol) in dry 1,4-dioxane (92 mL) was added pyridine (101.3 mmol) followed by a 2M solution of dimethylamine in THF (101.3 mmol). The reaction was allowed to warm to rt for 2 h, heated to 50 C for 1 h, then cooled to rt. After standing for 2 h, the precipitate was collected by filtration and rinsed with a minimal amount of cold water. Drying the precipitate to constant weight under high vacuum provided 14.1 g (55%) of the title compound as a white solid. MS (ES)+m/e 279.8, 282.0 [M+H]+.

1. temperatureheated to 50 C for 1 h
2. temperaturecooled to rt
3. filtrationthe precipitate was collected by filtration
4. washrinsed with a minimal amount of cold water
5. customDrying the precipitate to constant weight under high vacuum