Chlorosuccinimide → Ethyl 6-amino-5-chloronicotinate
反応式
[Cl:1]N1C(=O)CCC1=O.[CH2:9]([O:11][C:12](=[O:20])[C:13]1[CH:18]=[CH:17][C:16]([NH2:19])=[N:15][CH:14]=1)[CH3:10]>C(#N)C>[CH2:9]([O:11][C:12](=[O:20])[C:13]1[CH:18]=[C:17]([Cl:1])[C:16]([NH2:19])=[N:15][CH:14]=1)[CH3:10]参加物
4
実験手順
N-Chlorosuccinimide (21.7 g, 0.162 mol) was added to a suspension of 6-amino-nicotinic acid ethyl ester (18.0 g, 0.108 mol) in acetonitrile (270 ml) and the mixture was refluxed for 2 h. The reaction mixture was filtered and concentrated under reduced pressure. The residue was dissolved in dichloromethane, washed with water and dried. Flash chromatography (2.5% MeOH in CH2Cl2) gave pure 6-amino-5-chloro-nicotinic acid ethyl ester (17.23 g, 79%).
後処理
- temperaturethe mixture was refluxed for 2 h
- filtrationThe reaction mixture was filtered
- concentrationconcentrated under reduced pressure
- dissolutionThe residue was dissolved in dichloromethane
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-2ced570083014538a0270a15b33675f2
- 出典データセット
- uspto-grants-2006_07
- 特許番号
- US07071175B1
反応ノート
読み込み中…