反应详情

To a vigorously stirred solution of sodium bicarbonate (8.4 g, 100 mmol) and anhydrous sodium sulphite (12 g, 95 mmol) in water (50 ml) at 70°-80° C., was added naphthalene-1-sulphonyl chloride (11.5 g, 50 mmol) in portions and with vigorous stirring. The temperature was kept at 70°-80° C. by intermittent heating. When the addition was complete, the mixture was heated and stirred at 70°-80° C. for a further hour. The mixture was then allowed to cool to room temperature over 4 hours and acidified with 2M hydrochloric acid. The precipitated solid was collected by filtration, washed with water, air dried and then recrystallised from aqueous ethanol to give naphthalene-1-sulphinic acid as a solid (6.0 g), m.p. 86 87° C.

1. customwas kept at 70°-80° C. by intermittent heating
2. additionWhen the addition
3. temperaturethe mixture was heated
4. filtrationThe precipitated solid was collected by filtration
5. washwashed with water, air
6. customdried
7. customrecrystallised from aqueous ethanol