反应详情

温度

195 °C

A mixture of 5-(4-fluoro-benzyl)-[1,3,4]oxadiazol-2-ylamine 10.182 g (52.7 mmol), water 80 mL and anhydrous hydrazine 20 mL was refluxed under nitrogen on an oil bath (190-200 ° C.) for 23 hours. The mixture was cooled and allowed to crystallize at R.T. under nitrogen overnight. The precipitated product was collected by filtration, washed with ice-cold water (10 mL) and dried on high vacuum. The crude product was re-crystallized from water 60 mL (reflux under nitrogen, than to +4° C. in a refrigerator overnight). The product was filtered, washed with ice-cold water and dried on high vacuum. Y=6.210 g (56.5%) of a large white crystals. 1H-NMR(DMSO-d6, 400 MHz): 7.267 (app d, J=8.6 Hz, J=5.5 Hz, 2H), 7.097 (app t, J=9.0 Hz, 2H), 5.509 (br s, 2H), 5.339 (s, 2H), 3.884 (s, 2H); 19F-NMR(DMSO-d6, 376.5 MHz): −117.14 (m, 1F).

1. temperatureThe mixture was cooled
2. customto crystallize at R.T. under nitrogen overnight
3. filtrationThe precipitated product was collected by filtration
4. washwashed with ice-cold water (10 mL)
5. customdried on high vacuum
6. customThe crude product was re-crystallized from water 60 mL (
7. temperaturereflux under nitrogen, than to +4° C. in a refrigerator overnight)
8. filtrationThe product was filtered
9. washwashed with ice-cold water
10. customdried on high vacuum