Chlorosuccinimide → Ethyl 6-amino-5-chloronicotinate
반응식
[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]참가 물질
4
실험 절차
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%).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-2ced570083014538a0270a15b33675f2
- 출처 데이터셋
- uspto-grants-2006_07
- 특허 번호
- US07071175B1
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