Hydroxylamine → 3-Acetyl-isoquinoline oxime

HRID 932

반응식

HRID 932 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

반응물 3

HCID 787HydroxylamineHCID 517045Sodium AcetateHCID 112752751-(Isoquinolin-3-yl)ethan-1-one

생성물 1

HCID 1363959913-Acetyl-isoquinoline oxime수율 89%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

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

  1. temperaturewas heated
  2. temperatureto reflux for 1.5 hours
  3. extractionextracted with ethyl acetate
  4. customThe combined extracts were dried
  5. concentrationconcentrated
  6. customtriturated with hexane

출처 및 근거

ORD 기록
ord-6886621a94c642309e84fee2699ce813
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723473

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