反应详情

A solution of sodium hydroxide (8.0 gm, 0.2 ml) in methanol (170 mL) was added dropwise to a solution of 6-hydroxybenzothiazole-2-sulfonamide (23.0 gm, 0.1 mol) and allyl bromide (10.0 mL, 0.12 mol) in dry dimethylformamide (100 mL). This mixture was stirred at room temperature for 16-20 hours and then poured into hydrochloric acid-ice water. The precipitate was collected by filtration, dissolved in ethyl acetate, washed with water, dried (Na2SO4) and evaporated. This residue was triturated with methylene chloride and the crystalline product was collected. (wt. 9.9 gm), m.p. 184°-187° C. A sample was recrystallized from 1,2-dichloroethane, m.p. 193°-195° C.

1. filtrationThe precipitate was collected by filtration
2. dissolutiondissolved in ethyl acetate
3. washwashed with water
4. dry with materialdried (Na2SO4)
5. customevaporated
6. customThis residue was triturated with methylene chloride
7. customthe crystalline product was collected
8. customA sample was recrystallized from 1,2-dichloroethane, m.p. 193°-195° C.