تفاعل #324366

معادلة التفاعل

1,2,4,5-cyclohexanetetracarboxylic acid

acetic anhydride

→

1,2,4,5-cyclohexanetetracarboxylic dianhydride

المردود 96.7%

ظروف التفاعل

المعالجة

1. 1
   أخرىequipped with a Dimroth condenser
2. 2
   درجة الحرارةThe temperature was raised to the refluxing temperature of the solvent under a nitrogen gas atmosphere
3. 3
   درجة الحرارةto reflux for 10 min
4. 4
   أخرىwas decreased to room temperature
5. 5
   workup.STIRRINGunder stirring
6. 6
   أخرىto precipitate crystals
7. 7
   أخرىThe precipitated crystals were separated by solid-liquid separation
8. 8
   أخرىdried
9. 9
   أخرىto obtain primary crystals
10. 10
    أخرىThe mother liquor after separation
11. 11
    تركيزwas concentrated under reduced pressure
12. 12
    أخرىa rotary evaporator
13. 13
    أخرىto precipitate crystals
14. 14
    أخرىThe precipitated crystals were separated by solid-liquid separation
15. 15
    أخرىdried
16. 16
    أخرىto obtain secondary crystals

الإجراء التجريبي

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%).

المصدر