反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4](F)[N:3]=1.[NH:9]1[CH2:15][CH:14]([OH:16])[CH2:13][NH:12][CH2:11][CH2:10]1.CCN(C(C)C)C(C)C>C(O)C>[Br:1][C:2]1[N:3]=[C:4]([N:9]2[CH2:15][CH:14]([OH:16])[CH2:13][NH:12][CH2:11][CH2:10]2)[CH:5]=[CH:6][CH:7]=1参加物
5
反応条件
- 温度
- 100 °C
実験手順
A mixture of 2-bromo-6-fluoropyridine (477 mg, 2.7 mmol), 1,4-diazepan-6-ol (350 mg, 3 mmol), and DIPEA (1.94 g, 15 mmol) in ethanol (10 mL) was heated at 100° C. for 16 hours. After it was cooled, the reaction mixture was concentrated under reduced pressure. The residue was diluted with EtOAc (100 mL) and washed with brine. The organic layer was dried over Na2SO4 and concentrated under reduced pressure to afford 1-(6-bromopyridin-2-yl)-1,4-diazepan-6-ol as a colorless oil (400 mg, 48.9%). MS (ESI) m/z: 272 [M+H]+.
後処理
- temperatureAfter it was cooled
- concentrationthe reaction mixture was concentrated under reduced pressure
- additionThe residue was diluted with EtOAc (100 mL)
- washwashed with brine
- dry with materialThe organic layer was dried over Na2SO4
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-4a05fc6b800647e6bfba96bdba62fac7
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434725B2
関連ノート
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