Hydroxylamine → 3-Acetyl-isoquinoline oxime

HRID 932

反応式

HRID 932 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 1363959913-Acetyl-isoquinoline oxime収率 89%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6886621a94c642309e84fee2699ce813
出典データセット
uspto-grants-1998_03
特許番号
US05723473

関連ノート

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