Thionyl Chloride → 4,4-Difluorocyclohexane-1-carbonyl chloride
반응식
[F:1][C:2]1([F:11])[CH2:7][CH2:6][CH:5]([C:8](O)=[O:9])[CH2:4][CH2:3]1.S(Cl)([Cl:14])=O>C1(C)C=CC=CC=1>[F:1][C:2]1([F:11])[CH2:7][CH2:6][CH:5]([C:8]([Cl:14])=[O:9])[CH2:4][CH2:3]1참가 물질
4
실험 절차
4,4-Difluorocyclohexanecarboxylic acid (118.2 g, 0.72 mol) was dissolved in toluene (296 ml). To the clear solution was added thionyl chloride (261 ml, 3.6 mol) and the resultant solution was heated under reflux for 1.5 hours. A sample was taken and concentrated and 1H-NMR indicated complete conversion to the title compound. The reaction was cooled to room temperature and the thionyl chloride was removed under reduced pressure and replaced with toluene to give the title compound as a toluene concentrate at a total volume of 591 ml.
후처리
- temperatureunder reflux for 1.5 hours
- concentrationconcentrated
- customthe thionyl chloride was removed under reduced pressure
출처 및 근거
- ORD 기록
- ord-ac795bb4485843339eef8f4889f9c873
- 출처 데이터셋
- uspto-grants-2008_05
- 특허 번호
- US07368460B2
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