تفاعل #352851

معادلة التفاعل

hydrochloric acid

sodium hydroxide

trioctylamine

sodium methoxide

tetrafluorophthalic anhydride

→

3-methoxy-2,4,5-trifluorobenzoic acid

المردود 81.5%

المذيبات

xylene

methanol

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىInto a 100 ml glass reactor equipped with a reflux condenser and a stirrer
2. 2
   درجة الحرارةunder reflux
3. 3
   درجة الحرارةAfter cooling
4. 4
   درجة الحرارةThen, under reflux
5. 5
   workup.STIRRINGthe mixture was stirred for one hour
6. 6
   workup.STIRRINGthe mixture was stirred for 12 hors
7. 7
   درجة الحرارةunder reflux
8. 8
   درجة الحرارةAfter cooling
9. 9
   workup.STIRRINGthe mixture was stirred
10. 10
    أخرىThe organic layer was separated
11. 11
    workup.STIRRINGstirred at 140° C. for 2 hours
12. 12
    أخرىAfter completion of the reaction, 30 ml of a 20% sodium hydroxide aqueous solution
13. 13
    workup.ADDITIONwas added
14. 14
    workup.STIRRINGstirred
15. 15
    أخرىThe aqueous phase was separated
16. 16
    استخلاصextracted with ethyl acetate
17. 17
    workup.DISTILLATIONThe solvent was distilled off

الإجراء التجريبي

Into a 100 ml glass reactor equipped with a reflux condenser and a stirrer, 10 g (0.0397 mol) of the tetrafluorophthalic anhydride prepared in Example 3 and 20 ml of methanol were charged, and the mixture was stirred for 2 hours under reflux. After cooling, 42.8 g (0.079 mol) of a 10% methanol solution of sodium methoxide was dropwise added thereto. Then, under reflux, the mixture was stirred for one hour. Then, 15.9 g of a 10% sodium hydroxide aqueous solution was added thereto and the mixture was stirred for 12 hors under reflux. After cooling, 8 g of a 20 % hydrochloric acid aqueous solution was added. Further, 21.1 g (0.0596 mol) of trioctylamine and 40 g of xylene were added thereto, and the mixture was stirred. The organic layer was separated and stirred at 140° C. for 2 hours. After completion of the reaction, 30 ml of a 20% sodium hydroxide aqueous solution was added thereto and stirred. The aqueous phase was separated and neutralized with a 10% hydrochloric acid aqueous solution and extracted with ethyl acetate. The solvent was distilled off to obtain 6.7 g of 3-methoxy-2,4,5-trifluorobenzoic acid. The yield was 81.5%.

المصدر