3-Bromo-1,1,1-trifluoro-2-propanone → HCID 59334526, 화합물
반응식
[Br:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[CH:4][CH:3]=1.Br[CH2:10][C:11](=O)[C:12]([F:15])([F:14])[F:13]>C(O)C>[Br:1][C:2]1[N:7]2[CH:10]=[C:11]([C:12]([F:15])([F:14])[F:13])[N:8]=[C:6]2[CH:5]=[CH:4][CH:3]=1참가 물질
4
실험 절차
6-Bromopyridin-2-amine (20.0 g, 116 mmol) and 3-bromo-1,1,1-trifluoroacetone (24.0 mL, 231 mmol) were dissolved in ethanol (200 mL), and the mixture was heated under reflux for 4 days. The precipitated solid was collected by filtration and dissolved in dichloromethane. The solution was washed with saturated aqueous sodium hydrogen carbonate solution, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to give the title compound (26.0 g, yield 85%).
후처리
- temperaturethe mixture was heated
- temperatureunder reflux for 4 days
- filtrationThe precipitated solid was collected by filtration
- dissolutiondissolved in dichloromethane
- washThe solution was washed with saturated aqueous sodium hydrogen carbonate solution
- dry with materialdried over anhydrous sodium sulfate
- customthe solvent was evaporated under reduced pressure
출처 및 근거
- ORD 기록
- ord-6cc71be636dc4f66937d69d1b5e5f23f
- 출처 데이터셋
- uspto-grants-2012_02
- 특허 번호
- US08110585B2
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