関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Bromonaphthalene | HCID 11372 | — |
| 反応物 | 2-Bromoanthraquinone | HCID 221013 | — |
| 反応物 | HCID 178418306 | HCID 178418306 | — |
| 溶媒 | Pentane | HCID 8003 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Bromo-9,10-di-naphthalene-2-yl-9,10-dihydro-anthracene-9,10-diol | HCID 22247166 | 93% |
反応手順
To a solution of 2-bromonaphthalene (6.49 g, 31.3 mmol) in dry THF (50 ml) was added dropwise t-BuLi (18.4 ml of a 1.7 M solution in pentane) at −78° C. under nitrogen. After the mixture had been stirred for 30 min, 2-bromoanthraquinone (3.00 g, 10.4 mmol) was added at −78° C. The cooling bath was removed and the mixture was stirred for 2 hours at room temperature. The mixture was quenched with saturated aqueous ammonium chloride solution (50 ml) and extracted with ethyl ether (3×50 ml). The combined organic extracts were dried over MgSO4 and concentrated under vacuum. The crude product was slurried in petroleum ether, filtered off with suction, and washed with petroleum ether. After drying, the 2-bromo-9,10-di-naphthalene-2-yl-9,10-dihydro-anthracene-9,10-diol (5.30 g, 93%) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06998487B2 |
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| 出典データセット | uspto-grants-2006_02 |
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| ORD ID | ord-03bcbf3dd5ef4e5199d1c034360cbe7f |
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| 出典メモ | uspto-grants-2006_02 |
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