Pyridine → HCID 67454300、化合物
反応式
[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]=1参加物
5
実験手順
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).
後処理
- temperatureunder reflux
- concentrationwas concentrated
- custompurified on silica gel
出典と根拠
- ORDレコード
- ord-646eaa8e66ef488aa7137e19c8d57fa6
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08871761B2
反応ノート
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