関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phthalic Anhydride | HCID 6811 | — |
| 反応物 | 1,3-Difluorobenzene | HCID 9741 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | 1,1,1,2-Tetrachloroethane | HCID 12418 | — |
| 生成物 | 2-(2,4-difluorobenzoyl)benzoic Acid | HCID 7730336 | 75.3% |
反応手順
To a mixture of phthalic anhydride (64.8 g, 438 mmol), tetrachloroethane (600 mL) and 1,3-difluorobenzene (100 g, 877 mmol) was added anhydrous AlCl3 (141 g, 964 mmol) over 20 minutes while maintaining the reaction temperature below 40° C. The temperature was increased to 90° C. for 2 hours, the reaction mixture was cooled and poured into ice/6N HCl. The mixture was extracted with ether (2×1.2 L) and the combined ether extracts were dried over Na2SO4. The solvent was removed in vacuo and the residue was recrystallized from hot ethyl acetate to afford 86.5 g (75%) of 2-(2,4-difluorobenzoyl)benzoic acid, m.p. 129°-131° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05624922 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-9dfdf2457ad44b3da7dfaf12bb026b40 |
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| 出典メモ | uspto-grants-1997_04 |
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