Hydroxylamine → 3-Acetyl-isoquinoline oxime
반응식
[C:1]([C:4]1[N:5]=[CH:6][C:7]2[C:12]([CH:13]=1)=[CH:11][CH:10]=[CH:9][CH:8]=2)(=O)[CH3:2].[NH2:14][OH:15].C([O-])(=O)C.[Na+]>CO.O>[C:1](=[N:14][OH:15])([C:4]1[N:5]=[CH:6][C:7]2[C:12]([CH:13]=1)=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH3:2]참가 물질
6
실험 절차
A solution of 3-acetyl-isoquinoline (0.65 g), hydroxylamine (0.29 g) and sodium acetate (0.47 g) in a mixture of methanol (20 ml) and water (3 ml) was heated to reflux for 1.5 hours. The reaction was then poured into water and extracted with ethyl acetate. The combined extracts were dried, concentrated and triturated with hexane to give 3-acetyl-isoquinoline oxime (0.63, 89% yield) as a white crystalline solid m.p. 135°-142° C.; 1H NMR: 2.50(3H,s); 7.61(1H,t); 7.70(1H,t); 7.87(1H,d); 7.99(1H,d); 8.11(1H,s); 9.28(1H,s) ppm.
후처리
- temperaturewas heated
- temperatureto reflux for 1.5 hours
- extractionextracted with ethyl acetate
- customThe combined extracts were dried
- concentrationconcentrated
- customtriturated with hexane
출처 및 근거
- ORD 기록
- ord-6886621a94c642309e84fee2699ce813
- 출처 데이터셋
- uspto-grants-1998_03
- 특허 번호
- US05723473
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