Potassium Carbonate → 3-(4-Bromo-3,5-dimethylphenoxy)-1-methylpyrrolidin-2-one
반응식
[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([OH:9])=[CH:4][C:3]=1[CH3:10].Br[CH:12]1[CH2:16][CH2:15][N:14]([CH3:17])[C:13]1=[O:18].C([O-])([O-])=O.[K+].[K+]>CN(C)C=O>[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([O:9][CH:12]2[CH2:16][CH2:15][N:14]([CH3:17])[C:13]2=[O:18])=[CH:4][C:3]=1[CH3:10]참가 물질
5
실험 절차
To a solution of 4-bromo-3,5-dimethylphenol (100 mg) in N,N-dimethylformamide (2 mL) is added 3-bromo-1-methylpyrrolidin-2-one (100 mg) and K2CO3 (105 mg). The mixture is stirred for 12 hours at room temperature. Then the mixture is partitioned between water and diethylether. The organic phase is dried (MgSO4) and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 80:20→50:50) to give the title compound. Yield: 65 mg; LC (method 7): tR=1.0 min; Mass spectrum (ESI+): m/z=298 [M+H]+.
후처리
- customThen the mixture is partitioned between water and diethylether
- dry with materialThe organic phase is dried (MgSO4)
- concentrationconcentrated
- customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 80:20→50:50)
출처 및 근거
- ORD 기록
- ord-e9e8c9c3040d4ed78c35abd9e13ca709
- 출처 데이터셋
- uspto-grants-2014_02
- 특허 번호
- US08642585B2
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