反应详情

N,N-Dimethylformamide dimethyl acetal (1.5 mL, 11.3 mmol) was added to a partial suspension of 6-hydroxybenzothiazole-2-sulfonamide (2.3 gm, 10 mmol) in acetonitrile (20 mL) to give an immediate solution. After stirring at room temperature for 1 hour, the reaction mixture was cooled and the crystalline product which formed (1.95 gm) was collected m.p. 195°-198° C. Evaporation of the reaction solvent and dissolution of the residue in ethyl acetate/acetonitrile which was washed with water, dried (Na2SO4) and evaporated yielded an additional 0.6 gm from methylene chloride.

1. customto give an immediate solution
2. temperaturethe reaction mixture was cooled
3. customthe crystalline product which formed (1.95 gm)
4. customwas collected m.p. 195°-198° C
5. customEvaporation of the reaction solvent and dissolution of the residue in ethyl acetate/acetonitrile which
6. washwas washed with water
7. dry with materialdried (Na2SO4)
8. customevaporated
9. customyielded an additional 0.6 gm from methylene chloride