반응 #1028

ord-6886621a94c642309e84fee2699ce813

반응 방정식

CC(=O)c1cc2ccccc2cn1
3-acetyl-isoquinoline
NO
hydroxylamine
CC(=O)[O-].[Na+]
sodium acetate
CC(=NO)c1cc2ccccc2cn1
3-acetyl-isoquinoline oxime
수율 89.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도to reflux for 1.5 hours
  3. 3
    추출extracted with ethyl acetate
  4. 4
    기타The combined extracts were dried
  5. 5
    농축concentrated
  6. 6
    기타triturated with hexane

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723473uspto-grants-1998_03