関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Bromobenzene | HCID 7961 | — |
| 反応物 | Benzoyl chloride, 3-nitro- | HCID 8495 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 生成物 | 4-Bromo-3'-nitrobenzophenone | HCID 12321959 | 91.7% |
反応手順
In a 250 mL flask equipped with a nitrogen inlet, overhead stirring assembly, and reflux condenser were placed 3-nitrobenzoyl chloride (28 g, 0.15 mol), bromobenzene (130 g, 0.83 mol), and aluminum chloride (22 g, 0.16 mol). The mixture was heated for 3 h at 100° C., then cooled to room temperature and stirred for an additional 16 h. The mixture was poured into 1 L of acidic (HCl) ice water, and the organics were extracted using methylene chloride, dried over magnesium sulfate, and the solvents were removed under reduced pressure to yield a yellow powder. Recrystallization from acetone afforded 42.1 g (90% yield) of white crystals: m.p. 104°-105° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05412066 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-577526dbb11146de80d79d9d511240ce |
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| 出典メモ | uspto-grants-1995_05 |
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