反应 #1028

ord-6886621a94c642309e84fee2699ce813

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度to reflux for 1.5 hours
  3. 3
    萃取extracted with ethyl acetate
  4. 4
    其他The combined extracts were dried
  5. 5
    浓缩concentrated
  6. 6
    其他triturated with hexane

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723473uspto-grants-1998_03