2-Amino-5-bromo-3-methylpyridine → HCID 178422464、化合物
反応式
N[C:2]1[C:7]([CH3:8])=[CH:6][C:5]([Br:9])=[CH:4][N:3]=1.N([O-])=[O:11].[Na+]>OS(O)(=O)=O.O>[Br:9][C:5]1[CH:6]=[C:7]([CH3:8])[C:2]([OH:11])=[N:3][CH:4]=1参加物
5
実験手順
2-Amino-5-bromo-3-methylpyridine (5.0 g, 26.7 mmol) in 2.6M H2SO4 (70 mL) was treated with sodium nitrite (5.0 g, 72.5 mmol) in water (10 mL) dropwise at 0° C. The mixture was allowed to warm to ambient temperature and stir for 1.5 hours. The mixture was filtered and the filtercake washed with cold water. The filtercake was dissolved in dichloromethane (100 mL), dried (MgSO4), and concentrated to provide the title compound (4.2 g, 84% yield). MS (DCI/NH3) M/z 188/190 (M+H)+.
後処理
- filtrationThe mixture was filtered
- washthe filtercake washed with cold water
- dissolutionThe filtercake was dissolved in dichloromethane (100 mL)
- dry with materialdried (MgSO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-b215675b2fac4e29878af11d8c1f0757
- 出典データセット
- uspto-grants-2004_10
- 特許番号
- US06809105B2
反応ノート
読み込み中…