関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3-Bromotoluene | HCID 11560 | — |
| 反応物 | Cyclopropanecarbonyl chloride | HCID 77637 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 触媒 | Cadmium chloride, dihydrate | HCID 24633 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Cyclopropyl 3-methylphenyl ketone | HCID 21431776 | — |
反応手順
m-Bromotoluene (34.2 g) in dry ether (120 ml) was added dropwise to magnesium turnings (4.8 g) in dry ether (100 ml). The heat of reaction maintained the mixture to boiling under reflux during the addition and the mixture was heated under reflux for a further hour. The mixture was cooled to 0°, dry cadmium chloride (19.6 g) was added and the temperature allowed to rise to 20° C. After 1 hour, cyclopropanecarbonyl chloride (20.8 g) in dry ether (50 ml) was added dropwise and the mixture was heated under reflux for 4 hours, cooled to 0° and treated with 2 N hydrochloric acid. The ether layer was separated, washed with aqueous sodium bicarbonate (3× 100 ml., 8%) and with water, dried over magnesium sulphate, filtered and evaporated. The residue was distilled under reduced pressure and the fraction b.p. 86°-90°/0.4 mm was collected.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04028404 |
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| 出典データセット | uspto-grants-1977_06 |
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| ORD ID | ord-7b929bf6353d419388452c021da36ff0 |
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| 出典メモ | uspto-grants-1977_06 |
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