反应详情

0.60 mmol of 5-(N,N-diethylamino-2-ethyl)-4,7-dimethyl-1H-indole-2,3-dione hydrochloride (186.5 mg) and 0.70 mmol of (4-fluoro-benzyl)-[1,2,4]triazole-3,4-diamine (145 mg) in 1.5 mL of ethylene glycol was stirred at 125° C. for 1 day. The mixture was cooled to room temperature, diluted with water (5 mL), and neat diethylamine 0.5 mL was added. Stirred for 3 hours, the precipitate was collected by filtration, washed with water and dried on highvac. The obtained free base was suspended in water (10 mL), 2M HCl 0.5 mL was added, heated to boil, sonicated briefly while hot and then allowed to crystallize in a refrigerator (+5° C.) overnight. The precipitate was collected by filtration, washed with ice-cold water (2×1 mL) and dried on high vacuum.

1. additionwas added
2. filtrationthe precipitate was collected by filtration
3. washwashed with water
4. customdried on highvac
5. addition2M HCl 0.5 mL was added
6. temperatureheated
7. customsonicated briefly while hot and
8. customto crystallize in a refrigerator (+5° C.) overnight
9. filtrationThe precipitate was collected by filtration
10. washwashed with ice-cold water (2×1 mL)
11. customdried on high vacuum