関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Benzyl Chloride | HCID 7503 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sulfolane | HCID 31347 | — |
| 反応物 | 2,3,4-Trifluorophenol | HCID 123174 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | sodium 2-methylpropan-2-olate | HCID 178418730 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 溶媒 | Hexamethylphosphoramide | HCID 12679 | — |
| 溶媒 | 2(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl- | HCID 81646 | — |
| 生成物 | 1-(Benzyloxy)-2,3,4-trifluorobenzene | HCID 83396906 | — |
反応手順
2,3,4-Trifluorophenol was protected with hydroxy protection reagent (examples include BnBr, BnCl) at ambient temperature in the presence of base (include Na2CO3, K2CO3, NaHCO3, KHCO3, t-BuOK, t-BuONa) in appropriate inert solvent (include aliphatic and aromatic hydrocarbon (such as pentane, hexane, heptane, cyclohexane, petroleum ether, petrol, gasoline, benzene, toluene, xylene), aliphatic and aromatic halo-hydrocarbon (such as dichloromethane, 1,2-dichloroethane, chloroform, phenixin, chlorobenzene, o-dichlorobenzene), ether (such as diethyl ether, dibutyl ether, glycol dimethyl ether, 2-methoxyethyl ether, tetrahydrofuran, dioxane), ketone (such as acetone, methyl ethyl ketone, methyl isopropyl ketone, methyl isobutyl ketone), ester (such as ethyl acetate, methyl acetate), nitrile (such as acetonitrile, propiononitrile), amide (such as N,N-dimethylformamide, N,N-dimethylacetamide and N-methylpyrrolidin-2-one), DMSO, sulfolane, HMPA, DMPU, prefer acetone and methyl ethyl ketone). The reaction proceeds for several hours (3-12 h, prefer 5-10 h). 1-(Benzyloxy)-2,3,4-trifluorobenzene 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-7f32c74753794d89b4fd661dedd28682 |
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| 出典メモ | uspto-grants-2016_03 |
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