反应详情

温度

25 °C

To ammonium hydroxide (14.8M) (90 ml.) were added dropwise simultaneously sodium hypochlorite solution (5.25%) (42.4 ml.) and a solution of sodium hydroxide (1.2 g., 0.03 mole) and 2-mercapto-6-nitrobenzothiazole (6.37 g., 0.03 mole) in H2O (80 ml.) with stirring at <5° C. After 1/2 hr. the precipitated solid was collected by suction filtration and washed well with ice-H2O. The wet solid was suspended in acetone (120 ml.) with stirring at 25° C., treated with glacial acetic acid (2.4 ml.), then immediately treated dropwise wth 5% aqueous potassium permanganate solution (6.6 g, 0.04 mole in 120 ml H2O) over a 1/2 hr. period maintaining the reaction mixture temperature at <30° C. After stirring for an additional hour, the mixture was filtered to remove precipitated manganese dioxide, and the filtrate concentrated to remove the acetone and precipitate the solid product. Crystallization from 1,2-dichloroethane gave 1.18 g 6-nitro-2-benzothiazolesulfonamide, m.p. 176°-178° C. (dec).

1. filtrationthe precipitated solid was collected by suction filtration
2. washwashed well with ice-H2O
3. additiontreated with glacial acetic acid (2.4 ml.)
4. temperatureperiod maintaining the reaction mixture temperature at <30° C
5. stirringAfter stirring for an additional hour
6. filtrationthe mixture was filtered
7. customto remove
8. customprecipitated manganese dioxide
9. concentrationthe filtrate concentrated
10. customto remove the acetone
11. customprecipitate the solid product
12. customCrystallization from 1,2-dichloroethane