Piperidin-4-ol → HCID 67608386, 화합물
반응식
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]참가 물질
4
반응 조건
- 온도
- 150 °C
실험 절차
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]+.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-481ae1beaf2441ea995f657024da1cfd
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08822471B2
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