反应详情

温度

190 °C

A mixture of 4-(5-amino-[1,3,4]oxadiazol-2-ylmethyl)-phenol 4.902 g (25.64 mmol), water 40 mL and anhydrous hydrazine 13 mL was refluxed on an oil bath (190° C.) for 18 hours. The mixture was cooled, allowed to crystallize at room temperature for 2 hours, then placed into a freezer (−20° C.) overnight (16 hrs). The precipitated product was collected by filtration, washed with chilled MeOH (−15° C.) and dried on high vacuum. The crude product was re-crystallized from water (80 mL, reflux to +4° C. overnight). Filtered, washed with ice-cold water and dried on high vacuum.

1. temperatureThe mixture was cooled
2. customto crystallize at room temperature for 2 hours
3. customplaced into a freezer (−20° C.) overnight (16 hrs)
4. filtrationThe precipitated product was collected by filtration
5. washwashed with chilled MeOH (−15° C.)
6. customdried on high vacuum
7. customThe crude product was re-crystallized from water (80 mL, reflux to +4° C. overnight)
8. filtrationFiltered
9. washwashed with ice-cold water
10. customdried on high vacuum