関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2-Fluoropyridine | HCID 9746 | — |
| 反応物 | 1,4-Benzenedimethanol | HCID 11506 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (4-(Pyridin-2-yloxymethyl)-phenyl)-methanol | HCID 59255473 | 67.9% |
反応手順
To a mixture of 1,4-benzenedimethanol (5.5 g, 40 mmol), 2-fluoropyridine (1.3 g, 13 mmol), and N,N-dimethyl formamide (15 mL) was added sodium hydride (1.4 g, 40 mmol, 66% in oil) at 0° C, which was stirred at room temperature for 20 minutes and at 70° C for one hour. To the reaction mixture was added water, and extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride water, and the solvent thereof was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:1) to obtain the title compound (1.9 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08058444B2 |
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| 出典データセット | uspto-grants-2011_11 |
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| ORD ID | ord-e656e60029c0476ab312e1135b11d455 |
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| 出典メモ | uspto-grants-2011_11 |
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