참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Trioctylamine | HCID 14227 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Tetrafluorophthalic anhydride | HCID 69545 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 생성물 | 2,4,5-Trifluoro-3-methoxybenzoic acid | HCID 2733970 | 81.5% |
반응 단계
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%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05523476 |
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| 출처 데이터셋 | uspto-grants-1996_06 |
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| ORD ID | ord-04919f6c8d2544c5adf2e90f16b6d4f1 |
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| 출처 메모 | uspto-grants-1996_06 |
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