関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 9-Bromophenanthrene | HCID 11309 | — |
| 反応物 | HCID 178418306 | HCID 178418306 | — |
| 反応物 | HCID 178489586 | HCID 178489586 | — |
| 溶媒 | Pentane | HCID 8003 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 58238644 | HCID 58238644 | — |
反応手順
To a solution of 5.14 g (20.0 mmol) of 9-bromophenanthrene in 80 mL of THF, 26.7 mL (40.1 mmol) of 1.5 M tBuLi in pentane was added with vigorous stirring at −80° C. This mixture was additionally stirred for 1 hr at this temperature and then slowly warmed to room temperature. The resulting mixture was stirred for 30 min at ambient temperature and then cooled to −80° C. A solution of 4.22 g (20.0 mol) of 9 in 50 mL of THF was added. To the resulting mixture, 5 mL of water was added, and then this mixture was evaporated to dryness. The title product was isolated by flash chromatography on silica gel 60 (40-63 um, eluent: from hexanes to hexanes-diethyl ether=40:1, vol.). Yield 7.32 g (94%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08530593B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-fcd8a70a31eb43d696813268c1095200 |
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| 出典メモ | uspto-grants-2013_09 |
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