Chlorosuccinimide → 6-Bromo-5-chloropyridin-2-amine
反応式
[Br:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[CH:4][CH:3]=1.[Cl:9]N1C(=O)CCC1=O>C(#N)C.C(OCC)(=O)C>[Br:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[CH:4][C:3]=1[Cl:9]参加物
5
反応条件
- 温度
- 80 °C
実験手順
To a solution of 6-bromopyridin-2-amine (10 g, 58 mmol) in acetonitrile (150 mL) was added 1-chloropyrrolidine-2,5-dione (8.1 g, 60 mmol) and the mixture was heated at 80° C. for 10 hours. The mixture was diluted with ethyl acetate (200 mL) and washed with water. The organic phase was concentrated and purified by column chromatography (silica gel, 30% ethyl acetate in hexane) to afford the title compound. LCMS: 208 (M+H)+.
後処理
- washwashed with water
- concentrationThe organic phase was concentrated
- custompurified by column chromatography (silica gel, 30% ethyl acetate in hexane)
出典と根拠
- ORDレコード
- ord-96a9d554444142d3b6f9b07200c100d2
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09073922B2
反応ノート
読み込み中…