Methyl iodide → 5-Bromo-6-fluoro-1-methyl-1H-indazole
반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[NH:7][N:6]=[CH:5]2.[CH3:12]C([O-])(C)C.[K+].CI>CN(C=O)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[N:7]([CH3:12])[N:6]=[CH:5]2참가 물질
5
실험 절차
To a solution of 5-bromo-6-fluoro-1H-indazole (4 g, 18.60 mmol) in DMF (20 mL) was added potassium 2-methylpropan-2-olate (2.087 g, 18.60 mmol). The resulting mixture was stirred for 40 min. CH3I (3.17 g, 22.32 mmol) was added dropwise. After stirring overnight, the reaction mixture was quenched with NH4Cl (aq), extracted with EtOAc, washed with NH4Cl (aq), dried over Na2SO4, filtered and concentrated in vacuo to give a crude product, which was purified with silica gel column chromatography with gradient hexanes:EtOAc to give 5-bromo-6-fluoro-1-methyl-1H-indazole (1.86 g, 42%) as light yellow solid.
후처리
- stirringAfter stirring overnight
- customthe reaction mixture was quenched with NH4Cl (aq)
- extractionextracted with EtOAc
- washwashed with NH4Cl (aq)
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give a crude product, which
- customwas purified with silica gel column chromatography with gradient hexanes
출처 및 근거
- ORD 기록
- ord-6773249a0def4629bf59bf862b21d5e7
- 출처 데이터셋
- uspto-grants-2013_08
- 특허 번호
- US08507676B2
반응 노트
불러오는 중…