反应详情

To a solution of 1.5 g (7.1 mmoles) of 4-(1,2,4-triazol-1-ylmethyl)phenylamine hydrochloride in 3.75 ml of water and 6.3 ml of concentrated HCl, cooled to 0° C., was added slowly a solution of 0.5 g (7.2 mmoles) of sodium nitrite in 2.6 ml of water, keeping the temperature below 0° C. The mixture was stirred at this temperature for 15 minutes. Once this time had elapsed the solution of the diazonium salt was added rapidly to a solution of 5.37 g (42.6 mmoles) of sodium sulphite in 19 ml of water precooled to 0° C. under nitrogen atmosphere. The red solution was stirred at 0° C. for 10 minutes and then left to reach 65° C. in 1 hour. It was stirred at 65° C. for 30 minutes, and 5 ml of concentrated HCl were then added. The mixture was stirred at the same temperature under nitrogen atmosphere for 3 hours and then left to cool to room temperature.

1. customthe temperature below 0° C
2. customprecooled to 0° C. under nitrogen atmosphere
3. stirringThe red solution was stirred at 0° C. for 10 minutes
4. waitleft
5. waitto reach 65° C. in 1 hour
6. stirringIt was stirred at 65° C. for 30 minutes
7. stirringThe mixture was stirred at the same temperature under nitrogen atmosphere for 3 hours
8. waitleft