3-Bromo-1,1,1-trifluoro-2-propanone → HCID 59334526、化合物
反応式
[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]=1参加物
4
実験手順
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%).
後処理
- 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
出典と根拠
- ORDレコード
- ord-6cc71be636dc4f66937d69d1b5e5f23f
- 出典データセット
- uspto-grants-2012_02
- 特許番号
- US08110585B2
反応ノート
読み込み中…