関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2-(2-Bromoethyl)-1,3-dioxolane | HCID 87776 | — |
| 反応物 | 5,6-Difluoropyridin-3-ol | HCID 68430860 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-[2-(1,3-Dioxolan-2-yl)ethoxy]-2,3-difluoropyridine | HCID 68429762 | 38.1% |
反応手順
Cesium carbonate (33 g, 100 mmol) and 2-(2-bromoethyl)-1,3-dioxolane (12 g, 67 mmol) were added to an N,N-dimethylformamide suspension (30 ml) of 5,6-difluoropyridin-3-ol (8.8 g, 67 mmol), and stirred at 100° C. for 1 hour. The reaction solution was cooled to room temperature, water was added, and extracted with ethyl acetate. The organic layer was washed with saturated saline water, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane:chloroform=1:1 to 0:1) to obtain 5-[2-(1,3-dioxolan-2-yl)ethoxy]-2,3-difluoropyridine (5.9 g, yield: 38%) as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846700B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-9e72d3e1c42543f1aabdb607ad88b529 |
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| 出典メモ | uspto-grants-2014_09 |
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