Tetrahydrofuran → 1-(4-bromo-1H-pyrazol-1-yl)-2-methylbut-3-en-2-ol
반응식
[Br:1][C:2]1[CH:3]=[N:4][N:5]([CH2:7]C(=O)C)[CH:6]=1.[CH:11]([Mg]Br)=C.[CH2:15]1C[O:18][CH2:17][CH2:16]1>CCOC(C)=O>[Br:1][C:2]1[CH:3]=[N:4][N:5]([CH2:7][C:17]([CH3:11])([OH:18])[CH:16]=[CH2:15])[CH:6]=1참가 물질
5
실험 절차
To a cooled (0° C.) solution of 1-(4-bromo-1H-pyrazol-1-yl)propan-2-one (660 mg, 3.25 mmol) in THF (1 mL) was added vinyl magnesium bromide (1M in THF, 3.9 mL, 3.9 mmol) dropwise over 5 min. The resulting mixture was stirred for 1 h, diluted with 0.5 M HClaq and EtOAc and the layers separated. The organic phase was dried with MgSO4, filtered and concentrated in vacuo, then the crude residue was absorbed on silica gel and purified by column chromatography (0 to 100% EtOAc/Hex) to afford 1-(4-bromo-1H-pyrazol-1-yl)-2-methylbut-3-en-2-ol, MS ESI calcd. for C8H12BrN2O [M+H]+ 231. found 231.
후처리
- customthe layers separated
- dry with materialThe organic phase was dried with MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customthe crude residue was absorbed on silica gel
- custompurified by column chromatography (0 to 100% EtOAc/Hex)
출처 및 근거
- ORD 기록
- ord-dd5d698d5e2040c79378fda9dc25728b
- 출처 데이터셋
- uspto-grants-2016_01
- 특허 번호
- US09242984B2
반응 노트
불러오는 중…