반응 #623675

반응 방정식

2-chloro-5-fluoro-6-methylnicotinonitrile

hydrazine hydrate

diisopropyl ethylamine

water

→

5-Fluoro-6-methyl-1H-pyrazolo[3,4-b]pyridin-3-amine

용매

ethyl acetate

1,2-ethanediol

반응 조건

후처리

1. 1
   온도The reaction mixture was heated
2. 2
   온도After cooling
3. 3
   여과it was filtered with suction
4. 4
   기타The solid obtained
5. 5
   기타was dried
6. 6
   기타28.4 g (47% of theor.) of the target compound was obtained

실험 절차

58 g (340.027 mmol) of 2-chloro-5-fluoro-6-methylnicotinonitrile (preparation described in WO2007/41052, example U-2, page 80) was put in 1,2-ethanediol (580 ml) and then hydrazine hydrate (24.813 ml) and 56.091 ml (340.027 mmol) of diisopropyl ethylamine were added. The reaction mixture was heated with stirring for 16 h to 80° C. and then for 66 h to 120° C. After cooling, water (2.5 l) and ethyl acetate (2.5 l) were added and it was filtered with suction. The solid obtained was dried. 28.4 g (47% of theor.) of the target compound was obtained.

출처