참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | 4-Fluoroiodobenzene | HCID 9605 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 반응물 | HCID 178447999 | HCID 178447999 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | HCID 178447996 | HCID 178447996 | 40% |
반응 단계
Into a 300 cc four-necked flask, 5.59 g (25.2 mmol) of 4-fluroiodobenzene and 30 cc of dry ethyl ether were charged and cooled to -78° C. Then, 17 cc (27.8 mmol) of a n-hexane solution of n--C4H9Li (1.63 mol/l) was dropwise added thereto over a period of 15 minutes. Further, the mixture was stirred at -78° C. for one hour. Then, 3.8 cc (25.5 mmol) of N,N,N',N'-tetramethylene ethylenediamine was added thereto. Further, a dry diethyl ether (10 cc) solution containing 1.3 g (6.31 mmol) of 2-(trans-4-n-propylcyclohexyl)-1,1,2-trifluoroethylene obtained in Example 1, was dropwise added thereto over a period of 30 minutes. Further, the mixture was reacted at the same temperature for one hour, and then stirred at room temperature for one hour. Then, 50 cc of 1N hydrochloric acid was added thereto. The organic layer was separated. The aqueous layer was extracted with n-hexane, and the extract was combined with the organic layer. The combined organic layer was washed with water and dried. Further, the solvent was distilled off. The obtained crude solution was purified by silica gel column chromatography to obtain a solid. This solid was recrystallized from methanol to obtain 0.71 g (yield: 40%) of (E)-1-(4-fluorophenyl)-2-(trans-4-n-propylcyclohexyl)-1,2-difluoroethylene.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05621147 |
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| 출처 데이터셋 | uspto-grants-1997_04 |
|---|
| ORD ID | ord-c38ba36af653435db6a9be5af49de60e |
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| 출처 메모 | uspto-grants-1997_04 |
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