反应详情

13.5 g of 5-(dimethylsulphamoyl)-isatoic acid anhydride and 70 ml of absolute dioxane are gently warmed. As soon as the reaction mixture has reached 40°C, a solution of 8.3 g of N-methoxycarbonylpiperazine is added dropwise and the mixture is then heated further, an evolution of carbon dioxide setting in at about 70°C. The mixture is heated under reflux for a further hour and allowed to cool somewhat, insoluble matter is filtered off and the filtrate is concentrated under reduced pressure. The colourless crystals which are precipitated are filtered off with suction and recrystallised from 350 ml of methanol. 13.1 g of 1-[5-dimethylsulphamoyl)-anthraniloyl]-4-ethoxycarbonyl-piperazine, melting point 202°-204°C, are thus obtained.

1. customhas reached 40°C
2. temperaturethe mixture is then heated further
3. customin at about 70°C
4. temperatureThe mixture is heated
5. temperatureunder reflux for a further hour
6. temperatureto cool somewhat
7. filtrationinsoluble matter is filtered off
8. concentrationthe filtrate is concentrated under reduced pressure
9. customThe colourless crystals which are precipitated
10. filtrationare filtered off with suction
11. customrecrystallised from 350 ml of methanol