Piperidin-4-ol → HCID 67608386、化合物
反応式
Br[C:2]1[CH:7]=[N:6][C:5]([CH2:8][CH3:9])=[CH:4][N:3]=1.[OH:10][CH:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1>C(O)(C)C>[CH2:8]([C:5]1[N:6]=[CH:7][C:2]([N:14]2[CH2:15][CH2:16][CH:11]([OH:10])[CH2:12][CH2:13]2)=[N:3][CH:4]=1)[CH3:9]参加物
4
反応条件
- 温度
- 150 °C
実験手順
A mixture of 2-bromo-5-ethyl-pyrazine (1.66 g) and 4-hydroxy-piperidine (2.24 g) in isopropanol (15 mL) is heated to 150° C. overnight in an autoclave. After cooling to room temperature the solvent is evaporated in vacuo and water and dichloromethane are added. The aqueous phase is extracted with dichloromethane and the combined organic phases are washed with brine, dried over MgSO4 and concentrated in vacuo to give the title compound. LC (method 1): tR=0.66 min; Mass spectrum (ESI+): m/z=208 [M+H]+.
後処理
- temperatureAfter cooling to room temperature the solvent
- customis evaporated in vacuo and water and dichloromethane
- additionare added
- extractionThe aqueous phase is extracted with dichloromethane
- washthe combined organic phases are washed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-481ae1beaf2441ea995f657024da1cfd
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08822471B2
反応ノート
読み込み中…