関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Methyl chlorodifluoroacetate | HCID 73935 | — |
| 反応物 | Methyl 4-bromo-2-hydroxybenzoate | HCID 13983552 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl 4-bromo-2-(difluoromethoxy)benzoate | HCID 58959352 | 23% |
反応手順
To a 70 ml dimethylformamide solution of 5.0 g (21.7 mmol) of methyl 4-bromo-2-hydroxybenzoate, 3.4 ml (32.6 mmol) of methyl chlorodifluoroacetate and 3.0 g (21.7 mmol) of potassium carbonate were added. The mixture was stirred at 60° C. for 6 hours and at room temperature for 60 hours. Then, water was added to the reaction mixture, and the mixture was extracted with ether. The organic layer was washed with water and a saturated aqueous solution of sodium chloride. The washed system was dried over anhydrous sodium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=8/1) to obtain 1.4 g (23%) of the captioned compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07268128B2 |
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| 出典データセット | uspto-grants-2007_09 |
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| ORD ID | ord-e8a9a9e944ad4f3183cb5fe249758d1d |
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| 出典メモ | uspto-grants-2007_09 |
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