反应详情

温度

125 °C

According to the general cyclization procedure (for Example 27), 0.60 mmol of 4,7-dimethyl-1H-indole-2,3-dione (105 mg) and 0.70 mmol of (4-fluoro-benzyl)-[1,2,4]triazole-3,4-diamine (145 mg) in 2 mL of ethylene glycol was stirred at 125° C. overnight (18 hr). The mixture was cooled to room temperature, diluted with water (10 mL), stirred for 15 min. The precipitated product was collected by filtration, washed with MeOH+water 1:1. Dried on high vacuum. The crude product (187 mg) was suspended in anhydrous ethanol (6 mL), heated to reflux, sonicated while hot, allowed to cool overnight, filtered, washed with ice-cold methanol, filtered and dried on high vacuum.

1. temperatureThe mixture was cooled to room temperature
2. stirringstirred for 15 min
3. filtrationThe precipitated product was collected by filtration
4. washwashed with MeOH+water 1:1
5. customDried on high vacuum
6. temperatureheated
7. temperatureto reflux
8. customsonicated while hot,
9. temperatureto cool overnight
10. filtrationfiltered
11. washwashed with ice-cold methanol
12. filtrationfiltered
13. customdried on high vacuum