関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,6-Difluoropyridine | HCID 73934 | — |
| 反応物 | p-Cyanobenzyl alcohol | HCID 160549 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(6-Fluoro-pyridin-2-yloxymethyl)-benzonitrile | HCID 59255294 | 61% |
反応手順
To an N,N-dimethylformamide (50 mL) solution of 2,6-difluoropyridine (5 g, 43.4 mmol) and 4-(hydroxymethyl)benzonitrile (8.67 g, 65.1 mmol) was added sodium hydride (2.56 g, 65.1 mmol, 60% in oil) at room temperature. This mixture was stirred for 4 hours at 70° C. This mixture was partitioned into ethyl acetate and water. The organic layer was separated, washed with water, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by NH-silica gel column chromatography (heptane:ethyl acetate=10:1-4:1) to obtain the title compound (5.99 g, 61%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08841327B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-368df5206f534432a401e90a0dc900a3 |
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| 出典メモ | uspto-grants-2014_09 |
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