Piperidine → HCID 67187268, 화합물
반응식
F[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[C:7](=[O:12])[CH2:6][CH2:5]2.[NH:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1>N1C=CC=CC=1>[F:11][C:10]1[CH:9]=[C:8]2[C:4]([CH2:5][CH2:6][C:7]2=[O:12])=[CH:3][C:2]=1[N:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1참가 물질
4
실험 절차
5,6-difluoro-indan-1-one (2.49 g, 14.8 mmol) and piperidine (4.4 ml, 3.78 g, 44.4 mmol) were dissolved in pyridine (10 ml) and heated to reflux for 16 hours. The reaction was cooled, and the solvent removed under vacuum. The residue was taken in ethyl ether, washed with 1N aqueous sodium hydroxide and water, dried with magnesium sulfate, and the solvent removed under vacuum to give the desired product as 2.97 g of a black solid that was used without further purification. 1H NMR (300 MHz, CDCl3) 7.32 (d, 1H), 6.88 (d, 1H), 3.19 (m, 4H), 3.03 (m, 2H), 2.66 (m, 2H), 1.73 (m, 4H), 1.62 (m, 2H). MS (CSI) m/e 234 (M+H)+
후처리
- temperatureheated
- temperatureto reflux for 16 hours
- temperatureThe reaction was cooled
- customthe solvent removed under vacuum
- washwashed with 1N aqueous sodium hydroxide and water
- dry with materialdried with magnesium sulfate
- customthe solvent removed under vacuum
출처 및 근거
- ORD 기록
- ord-b394b8a175d84154a5a9758629da0424
- 출처 데이터셋
- uspto-grants-2013_07
- 특허 번호
- US08487116B2
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