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.C1C(=O)N([Br:19])C(=O)C1.C([O-])(O)=O.[Na+]>C(#N)C>[Br:19][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
5
反応条件
- 温度
- 23 °C
実験手順
To a solution of 3-trifluoromethyl-pyridin-2-ylamine (16.21 g, 100 mmol) in acetonitrile (300 mL) at 5° C. was added NBS (17.8 g, 100 mmol) and the mixture was stirred at 23° C. for 1 h. Poured onto ice and sat. NaHCO3 soln., extracted with EtOAc, washed with brine, dried over Na2SO4. Removal of the solvent in vacuum left a yellow solid. Silica gel & cotton wool column filtratation with DCM gave the product as a yellow solid (23.71 g, 98%). MS (ISP) 240.1 [(M+H)+].
後処理
- extraction, extracted with EtOAc
- washwashed with brine
- dry with materialdried over Na2SO4
- customRemoval of the solvent in vacuum
- waitleft a yellow solid
出典と根拠
- ORDレコード
- ord-f2cb82ac31a741c4b32633417e0495f9
- 出典データセット
- uspto-grants-2008_11
- 特許番号
- US07446113B2
反応ノート
読み込み中…