反应 #324366

反应方程式

1,2,4,5-cyclohexanetetracarboxylic acid

acetic anhydride

→

1,2,4,5-cyclohexanetetracarboxylic dianhydride

收率 96.7%

反应条件

后处理

1. 1
   其他equipped with a Dimroth condenser
2. 2
   温度The temperature was raised to the refluxing temperature of the solvent under a nitrogen gas atmosphere
3. 3
   温度to reflux for 10 min
4. 4
   其他was decreased to room temperature
5. 5
   workup.STIRRINGunder stirring
6. 6
   其他to precipitate crystals
7. 7
   其他The precipitated crystals were separated by solid-liquid separation
8. 8
   其他dried
9. 9
   其他to obtain primary crystals
10. 10
    其他The mother liquor after separation
11. 11
    浓缩was concentrated under reduced pressure
12. 12
    其他a rotary evaporator
13. 13
    其他to precipitate crystals
14. 14
    其他The precipitated crystals were separated by solid-liquid separation
15. 15
    其他dried
16. 16
    其他to obtain secondary crystals

实验过程

Subsequently, 450 g of the obtained 1,2,4,5-cyclohexanetetracarboxylic acid and 4,000 g of acetic anhydride were charged into a 5-L glass separable flask equipped with a Dimroth condenser. The inner atmosphere of the reactor was replaced with nitrogen gas under stirring. The temperature was raised to the refluxing temperature of the solvent under a nitrogen gas atmosphere to allow the solvent to reflux for 10 min. After that, the temperature was decreased to room temperature under stirring to precipitate crystals. The precipitated crystals were separated by solid-liquid separation and dried to obtain primary crystals. The mother liquor after separation was concentrated under reduced pressure using a rotary evaporator to precipitate crystals. The precipitated crystals were separated by solid-liquid separation and dried to obtain secondary crystals. In total of the primary and secondary crystals, 375 g of 1,2,4,5-cyclohexanetetracarboxylic dianhydride was obtained (yield of the dianhydride: 96.6%).

来源