関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Sulfolane | HCID 31347 | — |
| 反応物 | Lithium diisopropylamide | HCID 2724682 | — |
| 反応物 | 1-(Benzyloxy)-2,3,4-trifluorobenzene | HCID 83396906 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexamethylphosphoramide | HCID 12679 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 溶媒 | 2(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl- | HCID 81646 | — |
| 生成物 | 5-Benzoxy-2,3,4-trifluorobenzoic acid | HCID 89704915 | — |
反応手順
To a solution of 1-benzyloxy-2,3,4-trifluorobenzene in appropriate inert solvent (such as, but not limited to, aliphatic and aromatic hydrocarbon (such as pentane, hexane, heptane, cyclohexane, petroleum ether, petrol, gasoline, benzene, toluene, xylene), ether (such as diethyl ether, dibutyl ether, glycol dimethyl ether, 2-methoxyethyl ether, tetrahydrofuran, dioxane), sulfolane, HMPA, DMPU, prefer anhydrous THF, ethyl ether and dioxane) was added strong base (such as LDA, n-BuLi, LiHDMS) at low temperature (−50-−80° C., prefer −78° C.) under nitrogen atmosphere. The stirring was maintained at this temperature for several hours (such as 0.5-12 h, prefer 0.5-2 h). The mixture was transferred to a bottle with dry ice. The mixture is stirred for some time (such as 3-12 h, prefer 5-10 h). 5-Benzoxy-2,3,4-trifluorobenzoic acid is obtained after conventional workup.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09290468B2 |
|---|
| 出典データセット | uspto-grants-2016_03 |
|---|
| ORD ID | ord-f8dd96d010bb4bc1b057b85424419897 |
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| 出典メモ | uspto-grants-2016_03 |
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