関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Ethyl-2-fluoro-1,1'-biphenyl | HCID 1490326 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | HCID 178444488 | HCID 178444488 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178444483 | HCID 178444483 | 51.5% |
反応手順
4-Ethyl-2-fluorobiphenyl (13.0 gram) was added in one portion to a stirred suspension of aluminium trichloride (9.54 gram) in dichloromethane (30 ml), followed by a solution of trans-4-n-pentylcyclohexyl acetyl chloride (15 gram) in dichloromethane (30 ml), added dropwise over 30 minutes. After stirring at room temperature for 31/2 hours, the reaction mixture was poured onto ice (250 gram) and hydrochloric acid (25 ml) and the product was extracted with 350 ml and 250 ml portions of petroleum ether (boiling point 60°-80° C.). The combined extracts were washed with water (150 ml), dried over anhydrous sodium sulphate and evaporated to dryness. The residue (26.8 gram) was crystallised from industrial methylated spirits at 0° C. to give 13.2 gram (51.5% yield) 4-(trans-4-n-pentylcyclohexylacetyl)-2'-fluoro-4'-ethylbiphenyl, melting point 72°-73° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04695131 |
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| 出典データセット | uspto-grants-1987_09 |
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| ORD ID | ord-a48c5a2205d64bc589a453973ad18110 |
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| 出典メモ | uspto-grants-1987_09 |
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