反応 #709011

反応方程式

diisobutyl ketone

phenol

1,8-dichloroanthraquinone

→

1,8-diphenoxyanthraquinone

反応条件

後処理

1. 1
   温度the reaction mixture is heated
2. 2
   workup.DISTILLATIONDistillation of water commences at 155° C
3. 3
   workup.ADDITION67 g of potassium carbonate are added
4. 4
   温度The batch is then heated to 160° C. over 90 minutes
5. 5
   その他to react at this temperature for 1 hour
6. 6
   その他The reactor is then closed
7. 7
   温度heated to 175°-176° C.
8. 8
   workup.WAITkept at this temperature for 5 hours
9. 9
   温度After cooling to 30° C.
10. 10
    その他the solvent is removed by distillation
11. 11
    workup.ADDITIONTo the reaction mixture are added 3 ml of 50% sodium hydroxide solution

実験手順

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%.

出典