反応 #1028

反応方程式

3-acetyl-isoquinoline

hydroxylamine

sodium acetate

→

3-acetyl-isoquinoline oxime

収率 89.0%

溶媒

water

methanol

water

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度to reflux for 1.5 hours
3. 3
   抽出extracted with ethyl acetate
4. 4
   その他The combined extracts were dried
5. 5
   濃縮concentrated
6. 6
   その他triturated with hexane

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.

出典