関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Fuming sulfuric acid | HCID 24681 | — |
| 反応物 | 2-Benzoyl-4-tert-butylbenzoic acid | HCID 3106283 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,7-Di-t-butylanthraquinone | HCID 357626 | 138% |
反応手順
4-t-Butyl-2-benzoylbenzoic acid 4 (32.0 g, 95 mmol) was placed into a round-bottom flask and oleum (30%, 290 mL) was then added. The reaction mixture turned black and the reaction temperature was increased to 120° C. and stirred for 3 h. The mixture was then poured into ice. The aqueous mixture was extracted using CH2Cl2 (5×), dried over Na2SO4 and concentrated to give a dark solid. This solid was passed through a silica gel column using CH2Cl2 as eluent. After concentrating, the yellow-brown solid was recrystallized from hexane to give product as yellow crystals 21.0 g (69% yield). 1H NMR (CDCl3) δ(ppm): 1.42 (s, 18H), 7.80 (d, J=8.2 Hz, 1H), 7.81 (d, J=8.2 Hz), 8.20 (d, J=8.2 Hz, 1H),), 8.22 (d, J=8.2 Hz, 1H), 8.31 (s, 2H); 13C NMR (CDCl3): 31.01, 35.58, 123.83, 123.90, 127.17, 127.28, 131.08, 131.15, 131.34, 131.42, 133.40, 133.49, 157.94, 158.05, 182.76, 183.28,183.78
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06361887B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-b2d7745392be45f99609dc14471cb9a7 |
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| 出典メモ | uspto-grants-2002_03 |
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