関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Bromobenzyl bromide | HCID 68527 | — |
| 反応物 | 2-(N,N-Dimethylamino)methyl-6-hydroxytetralin | HCID 21939764 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-(4-Bromobenzyl)oxy-2-(N,N-dimethylamino)methyltetralin | HCID 18361535 | 37.3% |
反応手順
2-(N,N-Dimethylamino)methyl-6-hydroxytetralin (5.0 g; obtained in Reference Example 16) was dissolved in DMF (130 ml), to which was added 60% oily sodium hydride (1.46 g) at 0° C. The reaction mixture was warmed to room temperature, and stirred for 1 hour. This was again cooled to 0° C., to which was added a DMF solution (20 ml) of 4-bromobenzyl bromide (10.0 g). The reaction mixture was stirred at room temperature for 2 hours, and water was added thereto, which was then extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous sodium chloride solution, then dried, and concentrated. The residue was purified by alumina column chromatography (eluent: ethyl acetate/hexane=1/10) to obtain the entitled compound (3.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06310107B1 |
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| 出典データセット | uspto-grants-2001_10 |
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| ORD ID | ord-6e98dee0e6814b37ac858bc46a771f6a |
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| 出典メモ | uspto-grants-2001_10 |
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