反应详情

温度

50 °C

A mixture of 205 ml of glacial acetic acid, 160 ml of water and 40 ml of conc. HCl is initially taken and 23.4 g (0.11 mol) of 4-methyl-5-amino-1,1,3-trioxo-2,3-dihydro-1λ6 benz[d]isothiazole are introduced with stirring at 15°-20° C. 7.9 g (0.115 mol) of sodium nitrite are added dropwise to the resulting suspension at 5°-10° C. and it is stirred at 5° C. for 30 min. The diazonium salt, which is present as a suspension, is then added dropwise in portions to a solution of 19.1 g (0.115 mol) of potassium iodide in 170 ml of water which is warmed to 50° C., nitrogen being formed. After cooling to room temperature, the deposited product is isolated by filtering off with suction, washed with water and dried under reduced pressure at 50° C. 32.5 g (0.1 mol=91% of theory) of a solid of m.p.: 257°-258° C. are obtained. A combustion analysis gave an iodine content of 38.5% (theory 39.3%).

1. stirringit is stirred at 5° C. for 30 min
2. customnitrogen being formed
3. temperatureAfter cooling to room temperature
4. customthe deposited product is isolated
5. filtrationby filtering off with suction
6. washwashed with water
7. customdried under reduced pressure at 50° C
8. custom32.5 g (0.1 mol=91% of theory) of a solid of m.p.: 257°-258° C. are obtained