関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tert-Butylbenzene | HCID 7366 | — |
| 反応物 | 3-Chloropropionyl chloride | HCID 69364 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(4-T-Butylphenyl)-3-chloropropan-1-one | HCID 22228393 | 101.5% |
反応手順
To aluminum chloride (29.33 g, 220 mmol) in dichloromethane (300 mL) at 0° C. with stirring was added dropwise a solution of t-butyl benzene (31 mL, 200 mmol) and 3-chloropropionyl chloride (19 mL, 200 mmol) in dichloromethane. After the addition was complete, the reaction mixture was stirred from 0° C. to room temperature overnight. Then next morning, TLC indicated that all of the t-butyl benzene was consumed, and the reaction mixture was cooled to 0° C. With stirring, water (about 120 mL) in a dropwise fashion until the effervescence ceased. Finally, the layers were separated, and the organic layer was washed with water (3×150 mL) and then brine (1×150 mL). The dichloromethane layer was dried over magnesium sulfate, filtered, concentrated and pumped to dryness to afford the title compound as a light tan powder (45.6 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536166B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-d96dad5729ed4f93b056a8353edd9d2d |
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| 出典メモ | uspto-grants-2013_09 |
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