関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 15-Crown-5 | HCID 36336 | — |
| 反応物 | (1R,2S,4R,5S)-Bicyclo[2.2.1]heptane-2,5-diol | HCID 9989289 | — |
| 生成物 | (1R,2S,4R,5S)-5-(Benzyloxy)bicyclo[2.2.1]heptan-2-ol | HCID 10036335 | — |
反応手順
To a stirred solution of (1R,2S,4R,5S)-bicyclo[2.2.1]-heptane-2,5-diol (1.15 g, 8.97 mmol) and 15-crown-5 (0.054 mL, 0.269 mmol) in tetrahydrofuran (30.0 mL, 8.97 mmol) were added at 10° C. (ice/water bath) finely ground sodium hydroxide (2.15 g, 53.8 mmol) and 1-(bromomethyl)benzene (1.07 mL, 8.97 mmol). After stirring at 10° C. for 3 h, the mixture was stirred at ambient temperature overnight. The mixture was partitioned between EtOAc and water, and the organic portions were washed with brine, and conc. in vacuo. The crude product was purified by flash column chromatography (0 to 80% of ethyl acetate in hexanes). The title compound was obtained as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08686011B2 |
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| 出典データセット | uspto-grants-2014_04 |
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| ORD ID | ord-6a53e48d1cd7428eb757d87955dad714 |
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| 出典メモ | uspto-grants-2014_04 |
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