反应 #1026
ord-1c93b7108442465f805b25dd4eb5e4ed
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度to reflux for 8 hours
- 2萃取extracted with ethyl acetate
- 3其他The combined extracts were dried
- 4浓缩concentrated
- 5其他chromatographed
实验过程
A solution of 1-acetyl-isoquinoline (3.42 g), hydroxylamine (1.53 g) and sodium acetate (2.46 g) in a 3:1 mixture of methanol:water (80 ml) was heated to reflux for 8 hours then allowed to stand for 16 hours. The reaction mixture was then poured into water and extracted with ethyl acetate. The combined extracts were dried, concentrated and chromatographed using ethyl acetate:hexane 3:7 as the eluant to give 1-acetyl-isoquinoline oxime (1.87 g, 58% yield) as a white crystalline solid m.p. 154.4°-155.3° C.; 1H NMR: 2.50(3H,s); 7.58-7.73(3H,m); 7.85(1H,m); 8.55(1H,m); 8.57(1H,m); 8.66(1H,s) ppm.