関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Butyl bromide | HCID 8002 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Bromobenzyl alcohol | HCID 70119 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Bromo-4-(butoxymethyl)benzene | HCID 11402253 | 89% |
反応手順
To a solution of 4-bromobenzyl alcohol (10.0 g, 53.5 mmol) in N,N-dimethylformamide (200 mL) was added sodium hydride (3.08 g, 64.2 mmol, 50% in oil) at 0° C. This mixture was stirred for 5 minutes at 0° C., and 1-bromobutane (7.47 mL, 69.3 mmol) was added thereto at 0° C. This mixture was stirred for 40 minutes at room temperature and then stirred for 25 minutes at 70° C. The reaction solution was partitioned into water and ethyl acetate at 0° C. The organic layer was washed with water and saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under a reduced pressure. The residue was purified by silica gel column chromatography (heptane:ethyl acetate=20:1) to obtain the title compound (11.5 g, 89%).
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-c867eb8cb16542a4bd9127ec7ee7dbb3 |
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| 出典メモ | uspto-grants-2014_09 |
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