Pyridine → HCID 67454300, 화합물
반응식
[F:1][C:2]1[CH:11]=[C:10]([F:12])[CH:9]=[CH:8][C:3]=1[C:4](=[N:6][OH:7])[NH2:5].N1C=CC=CC=1.Cl[C:20](=O)[C:21]([O:23][CH2:24][CH3:25])=[O:22]>C(Cl)Cl>[F:1][C:2]1[CH:11]=[C:10]([F:12])[CH:9]=[CH:8][C:3]=1[C:4]1[N:5]=[C:20]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[O:7][N:6]=1참가 물질
5
실험 절차
To a solution of 2,4-difluoro-N′-hydroxybenzimidamide 5.2 (3.52 g, 33% purity, max. 7.2 mmol) and pyridine (2.32 mL, 28.7 mmol) in anhydrous CH2Cl2 under N2 was added ethyl chlorooxoacetate (1.27 g, 9.32 mmol) dropwise over 5 min at RT. The mixture was stirred under reflux. After 1 h30, the rxn mixt. was concentrated and purified on silica gel using CH2Cl2, furnishing 1.414 g of title product 5a as colorless oil. Yield: 1.414 g (78%). LCMS: P=94%, rt=4.21 nm, m/z=255, 277 (M+Na).
후처리
- temperatureunder reflux
- concentrationwas concentrated
- custompurified on silica gel
출처 및 근거
- ORD 기록
- ord-646eaa8e66ef488aa7137e19c8d57fa6
- 출처 데이터셋
- uspto-grants-2014_10
- 특허 번호
- US08871761B2
반응 노트
불러오는 중…