反应详情

A mixture of ammonium chloride (1.2 g), metallic iron powder (11 g), concentrated hydrochloric acid (0.05 ml), and water (30 ml) was heated on a steam bath. 4-(m-Chlorophenoxy)-3-nitro-5-sulphamyl-benzoic acid (3 g) was added while stirring, and the heating was continued for 6 hours. Then 1N sodium hydroxide (50 ml) was added, and the reaction mixture was filtered. The filter cake was washed twice with 1N sodium hydroxide (50 ml each time). The combined filtrates were adjusted to a pH of 2.5 by the addition of 4N hydrochloric acid. After cooling, the precipitated 3-amino-4-(m-chlorophenoxy)-5-sulphamyl-benzoic acid was collected by suction, and recrystallized from aqueous ethanol. The melting point was 239°-240°C.

1. temperaturewas heated on a steam bath
2. filtrationthe reaction mixture was filtered
3. washThe filter cake was washed twice with 1N sodium hydroxide (50 ml each time)
4. additionThe combined filtrates were adjusted to a pH of 2.5 by the addition of 4N hydrochloric acid
5. temperatureAfter cooling
6. customthe precipitated 3-amino-4-(m-chlorophenoxy)-5-sulphamyl-benzoic acid was collected by suction
7. customrecrystallized from aqueous ethanol