Trimethylamine → N-(5-bromo-4-methylpyridin-2-yl)methanesulfonamide
反応式
[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]=1参加物
5
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-e6ea66330efc4d8e98d63fafb5141d8a
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08158820B2
反応ノート
読み込み中…