참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 4-Ethyl-2-fluoro-1,1'-biphenyl | HCID 1490326 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 반응물 | HCID 178444488 | HCID 178444488 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 178444483 | HCID 178444483 | 51.5% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04695131 |
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| 출처 데이터셋 | uspto-grants-1987_09 |
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| ORD ID | ord-a48c5a2205d64bc589a453973ad18110 |
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| 출처 메모 | uspto-grants-1987_09 |
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