反应详情

To a mixture of 1N sodium hydroxide (60 ml) and aqueous methylamine (3.43 g containing 1.2 g of methylamine) 4-chloro-5-chlorosulphonyl-3-nitro-benzoic acid (9.3 g) was added in portions, while stirring and keeping the mixture at 0°-3° C. Then the reaction mixture was left standing until it had reached room temperature, after which the 4-chloro-5-methylsulphamyl-3-nitro-benzoic acid was precipitated by slow acidification with 4N hydrochloric acid. The precipitate was collected by suction and recrystallized from aqueous ethanol. The melting point was 228°-229° C.

1. additionwas added in portions
2. customat 0°-3° C
3. waitThen the reaction mixture was left
4. customhad reached room temperature
5. customafter which the 4-chloro-5-methylsulphamyl-3-nitro-benzoic acid was precipitated by slow acidification with 4N hydrochloric acid
6. customThe precipitate was collected by suction
7. customrecrystallized from aqueous ethanol