関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | 2-Bromo-1,4-difluorobenzene | HCID 67862 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 生成物 | 1-(4-Bromo-2,5-difluorophenyl)ethan-1-one | HCID 9991653 | 31% |
反応手順
Anhydrous aluminum chloride was mixed (5 grams, 37.5 millimoles, 2.4 equivalents) with 1-bromo-2,5 difluorobenzene in a dry, round-bottom flask blanketed with nitrogen and fitted with a condenser. The mixture was heated to 60° C. and acetyl chloride (1.7 milliliters, 23.3 millimole, 1.5. equivalents) was added by syringe. The wet yellow solid changed then into a scarlet solution and was heated at 90° C. for 1 hour. The reaction mixture was poured onto 38 grams of ice, HCl was added (3 milliliters, 37% concentration) and the mixture was extracted with ether. The crude material was dried over magnesium sulfate and evaporated down. The crude material was purified by column chromatography or distilled. The product (1.2 grams, 31%) was obtained as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07456156B2 |
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| 出典データセット | uspto-grants-2008_11 |
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| ORD ID | ord-691c1f6113b0420b857c2890349e606a |
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| 出典メモ | uspto-grants-2008_11 |
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