反应详情

温度

5 °C

To a flask equipped with a reflux condenser, a nitrogen inlet, and a mechanical stirrer is added 50 gm of cyanuric chloride, 191 mL of ODCB and 108.4 gm of aluminum chloride. The mixture is cooled in an ice-bath to 5° C. and 6.5 gm of concentrated HCl was added over a period of 20 minutes. The mixture was allowed to warm to room temperature, and stirred for 2 hours. It was cooled back to 5° C. and then 54.7 gm of o-xylene was slowly added over a period of 3 hours, while allowing the temperature to go up to 21° C. The mixture was stirred at room temperature for additional 16 hours. The reaction mixture was heated to about 63° C. and 34 gm of resorcinol was added over a period of about 30 minutes. The mixture was held at about 75° C. for 3 hours. It was then added to 500 mL water and ODCB distilled off azeotropically. The precipitated solid was filtered off and washed with water. The material was dried in a vacuum oven to give 96 gm of crude 2-(2,4-dihydroxyphenyl)-4,6-bis(3,4-dimethylphenyl)-1,3,5-triazine. The HPLC analysis showed it to contain about 5% of polyresorcinol-triazines and 10.7% tris-o-xylyl-triazine.

1. customTo a flask equipped with a reflux condenser, a nitrogen inlet, and a mechanical stirrer
2. temperatureto warm to room temperature
3. temperatureIt was cooled back to 5° C.
4. customto go up to 21° C
5. stirringThe mixture was stirred at room temperature for additional 16 hours
6. temperatureThe reaction mixture was heated to about 63° C.
7. waitThe mixture was held at about 75° C. for 3 hours
8. distillationdistilled off azeotropically
9. filtrationThe precipitated solid was filtered off
10. washwashed with water
11. customThe material was dried in a vacuum oven