Piperazine → 1-[4-(Trifluoromethyl)pyridin-2-yl]piperazine
反応式
Cl[C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][N:3]=1.[NH:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.C(N(CC)CC)C>CN(C=O)C>[F:9][C:8]([F:11])([F:10])[C:6]1[CH:5]=[CH:4][N:3]=[C:2]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[CH:7]=1参加物
5
実験手順
A solution of 2-chloro-4-(trifluoromethyl)pyridine (2.0 g, 11 mmol), piperazine (3 g, 30 mmol) and triethylamine (3.1 mL, 22 mmol) in DMF (10 mL) was heated at 100° C. overnight and concentrated in vacuo. The residue was purified by column chromatography on silica gel (EtOAc to EtOAc/MeOH/Et3N=9/1/0.5) to give 1.09 g (43%) of pure product. MS calculated for C10H12F3N3: (M+H) 232; found 232.1.
後処理
- concentrationconcentrated in vacuo
- customThe residue was purified by column chromatography on silica gel (EtOAc to EtOAc/MeOH/Et3N=9/1/0.5)
出典と根拠
- ORDレコード
- ord-8569c7eace6c4438b8f31b8a191ede0c
- 出典データセット
- uspto-grants-2008_11
- 特許番号
- US07449467B2
反応ノート
読み込み中…