Methyl iodide → Methyl 5-fluoro-3-methyl-2-nitrobenzoate
반응식
[F:1][C:2]1[CH:3]=[C:4]([CH3:14])[C:5]([N+:11]([O-:13])=[O:12])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].[C:15](=O)([O-])[O-].[Cs+].[Cs+].CI>CN(C=O)C.[Cl-].[Na+].O>[F:1][C:2]1[CH:3]=[C:4]([CH3:14])[C:5]([N+:11]([O-:13])=[O:12])=[C:6]([CH:10]=1)[C:7]([O:9][CH3:15])=[O:8]참가 물질
6
실험 절차
To a solution of (E1) and cesium carbonate (1.5 eq.) in DMF (0.25 M) at RT was added methyl iodide (1.0 eq.). After the mixture was stirred for 18 h, brine was added and the mixture was extracted with EtOAc. The organic phase was dried (Na2SO4) and concentrated under reduced pressure. The yellow solid was used in the next step without purification. 1H NMR (400 MHz, DMSO, 300K) δ 7.63 (2H, m), 3.83 (3H, s), 2.29 (3H, s).
후처리
- extractionthe mixture was extracted with EtOAc
- dry with materialThe organic phase was dried (Na2SO4)
- concentrationconcentrated under reduced pressure
- customThe yellow solid was used in the next step without purification
출처 및 근거
- ORD 기록
- ord-eb1d0b75953d4e298139b60ae155ebf8
- 출처 데이터셋
- uspto-grants-2011_12
- 특허 번호
- US08071623B2
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