Реакция #1028

Уравнение реакции

3-acetyl-isoquinoline

hydroxylamine

sodium acetate

→

3-acetyl-isoquinoline oxime

Выход 89.0%

Растворители

water

methanol

water

Условия реакции

Обработка

1. 1
   Температураwas heated
2. 2
   Температураto reflux for 1.5 hours
3. 3
   Экстракцияextracted with ethyl acetate
4. 4
   ДругоеThe combined extracts were dried
5. 5
   Концентрированиеconcentrated
6. 6
   Другоеtriturated with hexane

Методика

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.

Источник