Trimethylamine → N-(5-bromo-4-methylpyridin-2-yl)methanesulfonamide
반응식
[Br:1][C:2]1[C:3]([CH3:9])=[CH:4][C:5]([NH2:8])=[N:6][CH:7]=1.CN(C)C.[CH3:14][S:15](Cl)(=[O:17])=[O:16]>C(Cl)Cl>[Br:1][C:2]1[C:3]([CH3:9])=[CH:4][C:5]([NH:8][S:15]([CH3:14])(=[O:17])=[O:16])=[N:6][CH:7]=1참가 물질
5
실험 절차
5-Bromo-4-methylpyridin-2-amine (1.56 g) was dissolved in DCM (40 ml), trimethylamine (1.4 ml) added, followed by methanesulfonyl chloride (1.9 g) and the mixture stirred for 20 min. The solution was washed with water, dried (MgSO4) and evaporated. The residue was dissolved in THF, treated with TBAF, stirred for 16 h and evaporated. The residue was purified by chromatography on silica eluting with 27% EtOAc/isohexane. Yield 1.3 g. Carried forward to step (ii) without characterisation.
후처리
- washThe solution was washed with water
- dry with materialdried (MgSO4)
- customevaporated
- dissolutionThe residue was dissolved in THF
- additiontreated with TBAF
- stirringstirred for 16 h
- customevaporated
- customThe residue was purified by chromatography on silica eluting with 27% EtOAc/isohexane
출처 및 근거
- ORD 기록
- ord-e6ea66330efc4d8e98d63fafb5141d8a
- 출처 데이터셋
- uspto-grants-2012_04
- 특허 번호
- US08158820B2
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