反应详情

温度

100 °C

Into a 50-mL 3-necked round-bottom flask, was placed a solution of 6-bromo-3-ethyl-1-phenyl-1H-indazole (0.10 g, 0.33 mmol, 1.00 equiv) in toluene (20 mL), piperazine (0.14 g, 1.628 mmol, 2.00 equiv), Cs2CO3 (0.16 g, 5.00 mmol, 1.50 equiv), Pd(OAc)2 (20 mg, 0.09 mmol, 0.03 equiv), BINAP (20 mg, 0.03 mmol, 0.03 equiv). The resulting solution was stirred for 20 h at 100° C. in an oil bath. The solids were filtered out. The residue was applied onto a silica gel column with dichloromethane/methanol (20:1). The resulting residue (50 mg) was purified by Prep-HPLC with the following conditions (AGILENT Pre-HPLC (UV-Directed)): Column, SunFire Prep C18, 5 um, 19*100 mm; mobile phase, water with 0.05% TFA and MeOH (10% MeOH up to 55% in 2.5 min, hold 55% in 2.5 min, up to 100% in 0.1 min, hold 100% in 0.3 min, down to 10% in 0.1 min); Detector, UV254 nm to yield 3-ethyl-1-phenyl-6-(piperazin-1-yl)-1H-indazole as a yellow solid.

1. customInto a 50-mL 3-necked round-bottom flask, was placed
2. filtrationThe solids were filtered out
3. customThe resulting residue (50 mg) was purified by Prep-HPLC with the following conditions (AGILENT Pre-HPLC (UV-Directed))
4. waitmobile phase, water with 0.05% TFA and MeOH (10% MeOH up to 55% in 2.5 min
5. customin 2.5 min
6. waitup to 100% in 0.1 min
7. customin 0.3 min
8. waitdown to 10% in 0.1 min)