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F[C:2]1[CH:7]=[CH:6][C:5](/[C:8](/[F:20])=[C:9](/[C@H:11]2[CH2:16][CH2:15][C@H:14]([CH2:17][CH2:18][CH3:19])[CH2:13][CH2:12]2)\[F:10])=[CH:4][CH:3]=1.Cl.[CH2:22]1[CH2:26]OC[CH2:23]1>>[CH2:23]([C@H:2]1[CH2:7][CH2:6][C@H:5](/[C:8](/[F:20])=[C:9](/[C@H:11]2[CH2:16][CH2:15][C@H:14]([CH2:17][CH2:18][CH3:19])[CH2:13][CH2:12]2)\[F:10])[CH2:4][CH2:3]1)[CH2:22][CH3:26]참가 물질
반응 조건
- 온도
- -10 °C
실험 절차
Then, a mixed solution containing 1.3 g (6.31 mmol) of 2-(trans-4-n-propylcyclohexyl)-1,1,2-trifluoroethylene obtained in Example 1 and 10 ml of dry THF, was dropwise added thereto at the same temperature over a period of 15 minutes. The mixture was reacted at the same temperature for one hour and then the temperature was raised to -10° C. Then, 100 ml 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. Then, the solvent was distilled off, and the obtained crude solution was purified by silica gel column chromatography. The obtained solid was further recrystallized from ethanol to obtain 1.18 g (yield: 60%) of (E)-1,2-bis(trans-4-n-propylcyclohexyl)-1,2-difluoroethylene.
후처리
- additionwas dropwise added
- customThe mixture was reacted at the same temperature for one hour
- customThe organic layer was separated
- extractionThe aqueous layer was extracted with n-hexane
- washThe combined organic layer was washed with water
- customdried
- distillationThen, the solvent was distilled off
- customthe obtained crude solution
- customwas purified by silica gel column chromatography
- customThe obtained solid was further recrystallized from ethanol
출처 및 근거
- ORD 기록
- ord-1564235662c9419a825d50edec702130
- 출처 데이터셋
- uspto-grants-1997_04
- 특허 번호
- US05621147
연결된 노트
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