تفاعل #1026

معادلة التفاعل

1-acetyl-isoquinoline

hydroxylamine

sodium acetate

methanol

→

1-acetyl-isoquinoline oxime

المردود 58.0%

المذيبات

water

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto reflux for 8 hours
2. 2
   استخلاصextracted with ethyl acetate
3. 3
   أخرىThe combined extracts were dried
4. 4
   تركيزconcentrated
5. 5
   أخرىchromatographed

الإجراء التجريبي

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.

المصدر