関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Xylyl bromide | HCID 7721 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-hydroxy-6,7,8,9-tetrahydro-5H-benzo[7]annulen-5-one | HCID 229507 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 22990062 | HCID 22990062 | 98% |
反応手順
To 3-hydroxy-5-oxo-6,7,8,9-tetrahydro-5H-benzocycloheptene (1.76 g, 10.0 mmol) dissolved in DMF (10 ml) were added potassium carbonate (2.76 g, 20.0 mmol) and 4-methylbenzyl bromide (2.04 g, 11.0 mmol), and the resulting mixture was stirred at room temperature for 24 hours. The reaction mixture was concentrated under reduced pressure, and the residue was mixed with water (20 ml) and extracted with ethyl acetate (20 ml×3). The combined organic layers were dried with anhydrous magnesium sulfate and were then concentrated under reduced pressure, and the residue was subjected to column chromatography (silica gel: 40 g, ethyl acetate/hexane=1/30). The objective fractions were concentrated under reduced pressure to obtain 3-(4-methylbenzyloxy)-5-oxo-6,7,8,9-tetrahydro-5H-benzocycloheptene (2.74 g, 9.77 mmol, 98%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06627651B1 |
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| 出典データセット | uspto-grants-2003_09 |
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| ORD ID | ord-bf545804ba4b47a0a1e3256006012525 |
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| 出典メモ | uspto-grants-2003_09 |
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