Methyl iodide → 3-Bromo-1,6-dimethylpyridin-2(1H)-one
반응식
[Br:1][C:2]1[C:3]([OH:9])=[N:4][C:5]([CH3:8])=[CH:6][CH:7]=1.[H-].[Na+].[Br-].[Li+].I[CH3:15]>C1COCC1.C(Cl)Cl>[Br:1][C:2]1[C:3](=[O:9])[N:4]([CH3:15])[C:5]([CH3:8])=[CH:6][CH:7]=1참가 물질
7
실험 절차
3-Bromo-6-methylpyridine-2-ol (2 g, 10.6 mmol) was taken up in THF and stirred. Sodium hydride (60% in oil 510 mg, 12.7 mmol) was added portion wise then stirred 30 minutes. Lithium bromide (1.85 g, 21.2 mmol) was added and stirred for 1 hour. Then iodomethane (1.32 mL, 21.2 mmol) was added and the reaction mixture was stirred overnight. The reaction mixture was diluted with DCM and washed with 1N NaOH. The DCM layer was dried over magnesium sulfate, filtered and dried in vacuo to afford 1.19 g product carried on to next step as is. LRMS (ESI) m/z 202/204 [(M+H)]+, calc'd for C7H8BrNO: 202.05.
후처리
- stirringstirred 30 minutes
- stirringstirred for 1 hour
- stirringthe reaction mixture was stirred overnight
- washwashed with 1N NaOH
- dry with materialThe DCM layer was dried over magnesium sulfate
- filtrationfiltered
- customdried in vacuo
출처 및 근거
- ORD 기록
- ord-165c9804823f463082a530b6e97ed2de
- 출처 데이터셋
- uspto-grants-2015_03
- 특허 번호
- US08969565B2
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