N-bromobutanimide → 5-Bromo-3-(trifluoromethyl)pyridin-2-amine
反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[C:4]([NH2:9])=[N:5][CH:6]=[CH:7][CH:8]=1.[Br:12]N1C(=O)CCC1=O>CC#N>[Br:12][C:7]1[CH:8]=[C:3]([C:2]([F:1])([F:10])[F:11])[C:4]([NH2:9])=[N:5][CH:6]=1参加物
4
実験手順
To a solution of 3-trifluoromethyl-pyridin-2-ylamine (Fluorochem Ltd., Derbyshire, United Kingdom, 5.37 g, 32.8 mmol) in 100 ml of dry CH3CN under argon were added N-bromosuccinimide (6.45 g, 36.2 mmol) in 4 equal portions over a period of 1 h at 0-5° C. The cooling bath was removed and stirring was continued for 3 h. The solvent was evaporated under vacuum, then the residue was dissolved in EtOAc and washed with water and brine. The organic layer was dried over Na2SO4 and evaporated to give the title compound as a orange oil. (M+H=239; 241).
後処理
- customThe cooling bath was removed
- customThe solvent was evaporated under vacuum
- dissolutionthe residue was dissolved in EtOAc
- washwashed with water and brine
- dry with materialThe organic layer was dried over Na2SO4
- customevaporated
出典と根拠
- ORDレコード
- ord-f6d7c9ae79934660842df9765f08cf0f
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08476294B2
反応ノート
読み込み中…