反应详情

温度

35 °C

A stirred pressure reactor is charged with 183 ml of diisobutyl ketone. With stirring, 86.3 g of phenol (90%) are added. Then 103.8 g of 1,8-dichloroanthraquinone are added over 5 minutes and the reaction mixture is heated to boiling point. Distillation of water commences at 155° C. After 1.5 hours at this temperature, the reaction mixture is cooled to 35° C. and then 67 g of potassium carbonate are added. The batch is then heated to 160° C. over 90 minutes and allowed to react at this temperature for 1 hour. The reactor is then closed, heated to 175°-176° C. and kept at this temperature for 5 hours. After cooling to 30° C., the pressure in the reactor is reduced and the solvent is removed by distillation. To the reaction mixture are added 3 ml of 50% sodium hydroxide solution and the resultant 1,8-diphenoxyanthraquinone is isolated by filtration and vacuum dried, to give 141.0 g of a product with a titre of 86.2%, corresponding to a yield of 89.0%. The conversion is 99.9%.

1. temperaturethe reaction mixture is heated
2. distillationDistillation of water commences at 155° C
3. addition67 g of potassium carbonate are added
4. temperatureThe batch is then heated to 160° C. over 90 minutes
5. customto react at this temperature for 1 hour
6. customThe reactor is then closed
7. temperatureheated to 175°-176° C.
8. waitkept at this temperature for 5 hours
9. temperatureAfter cooling to 30° C.
10. customthe solvent is removed by distillation
11. additionTo the reaction mixture are added 3 ml of 50% sodium hydroxide solution