Hydroxyamine hydrochloride → 2-Chloro-3-fluoro-pyridine-4-carbaldehyde oxime
반응식
[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]=1참가 물질
6
실험 절차
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.
후처리
- concentrationThe reaction mixture was concentrated in vacuo
- filtrationThe precipitate was filtered off
- washwashed with CH2Cl2
- customdried
출처 및 근거
- ORD 기록
- ord-a4d4d9bdaf8a402aaa9560ba77a6b369
- 출처 데이터셋
- uspto-grants-2015_07
- 특허 번호
- US09085555B2
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