関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenol | HCID 996 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2-Bromo-3,4-dihydro-7-methoxy-1(2H)-naphthalenone | HCID 311906 | — |
| 触媒 | Cesium iodide | HCID 24601 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 3,4-Dihydro-7-methoxy-2-phenoxy-1(2H)-naphthalenone | HCID 19600662 | 61% |
反応手順
A mixture of 2.95 g (31.4 mmol) of phenol, 25.5 g (78.2 mmol) of cesium carbonate and 320 mg (1.23 mmol) of cesium iodide in 64 ml of acetone was heated at reflux for 40 minutes and then cooled to 0° C. To this 0° C. mixture was added 8.00 g (31.4 mmol) of 2-bromo-3,4-dihydro-7-methoxy-1(2H)-naphthalenone. The resultant reaction mixture was stirred 3 hours at 0° C. and 15 hours at 25° C., then filtrated. The filtrate was evaporated to an oil which was purified via column chromatography on 400 g of silica gel, eluting with 25% ether-hexane, to give 5.14 g (61%) of present title product as an oil, crystallized from ether-hexane, m.p. 94.5°-96.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05059609 |
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| 出典データセット | uspto-grants-1991_10 |
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| ORD ID | ord-247c94125d3645308c0867241150d39c |
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| 出典メモ | uspto-grants-1991_10 |
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