Hydroxyamine hydrochloride → 2-Chloro-3-fluoro-pyridine-4-carbaldehyde oxime
反応式
[Cl:1][C:2]1[C:7]([F:8])=[C:6]([CH:9]=O)[CH:5]=[CH:4][N:3]=1.Cl.[NH2:12][OH:13].C([O-])(=O)C.[NH4+]>CO.O>[Cl:1][C:2]1[C:7]([F:8])=[C:6]([CH:9]=[N:12][OH:13])[CH:5]=[CH:4][N:3]=1参加物
6
実験手順
To a solution of 2-chloro-3-fluoro-pyridine-4-carbaldehyde (1.20 g, 5.64 mmol) in MeOH (48 mL) and water (8 mL) were added hydroxylamine hydrochloride (0.59 g, 8.46 mmol) and ammonium acetate (1.30 g, 16.9 mmol), and stirring was continued at RT overnight. The reaction mixture was concentrated in vacuo, and the residue was suspended in CH2Cl2/MeOH 9:1. The precipitate was filtered off, washed with CH2Cl2 and dried to afford the title compound as a white solid. MS (LC/MS): 175.0 [M+H]+; tR (HPLC conditions b): 2.78 min.
後処理
- concentrationThe reaction mixture was concentrated in vacuo
- filtrationThe precipitate was filtered off
- washwashed with CH2Cl2
- customdried
出典と根拠
- ORDレコード
- ord-a4d4d9bdaf8a402aaa9560ba77a6b369
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09085555B2
反応ノート
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