1,3-Dibromo-5,5-dimethylhydantoin → 3-bromo-N-methylpyridin-4-amine
反応式
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=1.[Br:9]N1C(C)(C)C(=O)N(Br)C1=O>O1CCCC1>[Br:9][C:4]1[CH:5]=[N:6][CH:7]=[CH:8][C:3]=1[NH:2][CH3:1]参加物
4
実験手順
To a solution of 10.6 g (98 mmol) 4-(N-methylamino)-pyridine in 200 ml tetrahydrofuran was added dropwise a solution of 14.0 g (49 mmol) 1,3-dibromo-5,5-dimethylhydantoin in 50 ml tetrahydrofuran at room temperature within 1.5 h. The solvent was removed and the residue was re-dissolved in ethyl acetate. The organic phase was washed four times with saturated sodium carbonate solution, dried (sodium sulfate) and evaporated. The residue was purified by flash chromatography to give 10.3 g (56%) of the title compound as white crystals.
後処理
- customThe solvent was removed
- dissolutionthe residue was re-dissolved in ethyl acetate
- washThe organic phase was washed four times with saturated sodium carbonate solution
- dry with materialdried (sodium sulfate)
- customevaporated
- customThe residue was purified by flash chromatography
出典と根拠
- ORDレコード
- ord-89fe98bd4d8f4af48daafe991e54740f
- 出典データセット
- uspto-grants-2001_05
- 特許番号
- US06225316B1
反応ノート
読み込み中…