関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trimethylsilyl cyanide | HCID 82115 | — |
| 反応物 | 4-[(5,6,7,8-Tetrahydro-8,8-dimethyl-5-oxonaphth-3-yl)ethynyl]benzoic acid | HCID 18314593 | — |
| 触媒 | zinc(II)iodide | HCID 9883512 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-[(7,8-Dihydro-8,8-dimethyl-5-trimethylsiloxynaphth-3-yl)ethynyl]benzoic acid | HCID 19962311 | — |
反応手順
To a cold solution (0° C.) of 50 mg (0.07 mmol) of zinc iodide (dried in vacuo over P2O5 for several hours) in 2 ml of dry THF (flushed with argon) was added a solution of 0.110 g (0.34 mmol) of 4-[(5,6,7,8-tetrahydro-8,8-dimethyl-5-oxonaphth-3-yl)ethynyl]benzoic acid (Compound 8) in 2 ml of THF followed by 0.14 ml (1.03 mmol) of cyanotrimethylsilane. The resulting mixture was stirred at 25° C. for 12 hours and purified by flash chromatography (silica, 50% EtOAc-hexane) to yield the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05618931 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-35939b1acb954bdebea6354ff1e69bdf |
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| 出典メモ | uspto-grants-1997_04 |
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