反应详情

Neutralization of the hydrazine hydrochloride of Example 2 was effected by stirring with 19.6 g (0.21 mol) sodium bicarbonate in 100 ml isopropanol. When gas evolution ceased (1 1/2hours) the system was cooled in an ice-water bath, and 25 g (0.1 mol) 3-sulfamoyl-4-chlorobenzoyl chloride was added in several portions. Throughout this addition the temperature was maintained between 5° and 20° C. After the addition the reaction mixture was stirred at room temperature overnight. The reaction mixture was then cooled to 0°-5° C., diluted with 80 ml water, and stirred for 2 more hours.

1. custom(1 1/2hours)
2. temperaturewas cooled in an ice-water bath
3. additionThroughout this addition the temperature
4. temperaturewas maintained between 5° and 20° C
5. additionAfter the addition the reaction mixture
6. temperatureThe reaction mixture was then cooled to 0°-5° C.
7. stirringstirred for 2 more hours