Dimethylformamide → 5-Bromo-3-chloropyridin-2-amine
反応式
[Cl:1]N1C(=O)CCC1=O.CN(C)C=O.[Br:14][C:15]1[CH:16]=[CH:17][C:18]([NH2:21])=[N:19][CH:20]=1.[OH-].[Na+]>O>[Br:14][C:15]1[CH:16]=[C:17]([Cl:1])[C:18]([NH2:21])=[N:19][CH:20]=1参加物
6
実験手順
With cooling with ice, 1-chloropyrrolidine-2,5-dione (10 g, 76 mmol) was added to an N,N-dimethylformamide solution (30 ml) of 5-bromopyridine-2-amine (12 g, 69 mmol), and stirred for 4 hours. The reaction solution was diluted with water, neutralized with aqueous 5 N sodium hydroxide solution, and extracted with diethyl ether. The organic layer was washed with saturated saline water, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane:chloroform:ethyl acetate=25:25:50) to obtain 5-bromo-3-chloropyridine-2-amine (12.6 g, yield: 88%) as a brown solid.
後処理
- extractionextracted with diethyl ether
- washThe organic layer was washed with saturated saline water
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe obtained residue was purified by silica gel column chromatography (hexane:chloroform:ethyl acetate=25:25:50)
出典と根拠
- ORDレコード
- ord-a17d1aed286040c38f0b034b4b075e95
- 出典データセット
- uspto-grants-2012_07
- 特許番号
- US08232284B2
反応ノート
読み込み中…