反应详情

A suspension of 88.1 g of 4-nitro-4'-(dimethylamino)azobenzene in 1080 ml of ethanol was heated to slight reflux while stirring, treated dropwise within 35 minutes with 1017 g of 25% sodium hydrogen sulphide solution and then stirred at slight reflux for another 1 hour. The mixture was cooled to room temperature, treated with 2120 ml of water and suction filtered. The residue was washed with water/ethanol (vol. 3:1) and dried at 50° C. in vacuo, yielding 55.7 g of 4-amino-4'-(dimethylamino)azobenzene; m.p. 182.5°-187.4° C.

1. temperaturewas heated
2. temperatureto slight reflux
3. stirringstirred
4. temperatureat slight reflux for another 1 hour
5. filtrationfiltered
6. washThe residue was washed with water/ethanol (vol. 3:1)
7. customdried at 50° C. in vacuo