6-Amino-3-chloropyridazine → 3-Amino-4-bromo-6-chloropyridazine
反応式
[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH2:8])=[CH:4][CH:3]=1.C([O-])(O)=O.[Na+].[Br:14]Br>CO>[Br:14][C:4]1[CH:3]=[C:2]([Cl:1])[N:7]=[N:6][C:5]=1[NH2:8]参加物
5
実験手順
To a solution of 6-Chloro-pyridazin-3-ylamine (4 g, 31 mmol) in methanol (60 mL) was added NaHCO3 (5.2 g, 62 mmol). The reaction mixture was stirred for 30 minutes at RT then Br2 (4.9 g, 31 mmol) was added drop wise. Then the resulting reaction mixture was stirred additionally for 16 h at RT. After completion of reaction, the reaction mass concentrated under reduced pressure, crude purified by silica gel (100-200 mesh) chromatography using EtOAc/Hexane (8:2) to afford 4-Bromo-6-chloro-pyridazin-3-ylamine (2.3 g, 36%) as a solid.
後処理
- customThen the resulting reaction mixture
- stirringwas stirred additionally for 16 h at RT
- customAfter completion of reaction
- concentrationthe reaction mass concentrated under reduced pressure, crude
- custompurified by silica gel (100-200 mesh) chromatography
出典と根拠
- ORDレコード
- ord-4e3baff1832d4fa7abb52f3c6518eb96
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08822457B2
反応ノート
読み込み中…