反应详情

温度

0 °C

0.32 g (0.62 mmol) 2-{[2-((E)-{4-[ethyl(2-hydroxyethyl)amino]phenyl}-diazenyl)-4-(1-piperidinyl)-1,3-thiazol-5-yl]methylene}-1H-indene-1,3(2H)-dione were dissolved in 33 ml THF and cooled to 0° C. Then 0.11 g (0.93 mmol) chlorosulfonic acid were added slowly drop by drop with stirring. After the addition was completed, the reaction mixture was heated under reflux for 4 hours, allowed to cool to room temperature and stirred overnight. After further cooling in an ice bath the formed precipitate was filtered off, washed with a little cold THF and dried at 40° C. in vacuum.

1. additionAfter the addition
2. temperaturethe reaction mixture was heated
3. temperatureunder reflux for 4 hours
4. temperatureto cool to room temperature
5. stirringstirred overnight
6. temperatureAfter further cooling in an ice bath the formed precipitate
7. filtrationwas filtered off
8. washwashed with a little cold THF
9. customdried at 40° C. in vacuum