反应详情

温度

100 °C

1-[3-({[tert-Butyl(dimethyl)silyl]oxy}methyl)-2-fluorophenyl]piperazine (400 mg) was suspended in toluene (8 ml), and 3-chloropyridazine hydrochloride (242 mg), Pd2(dba)3(56 mg), dicyclohexyl(2′,6′-dimethoxybiphenyl-2-yl)phosphine (51 mg), and sodium tert-butoxide (308 mg) were added thereto, followed by stirring at 100° C. overnight. The reaction mixture was cooled to room temperature, and filtered by the addition of CHCl3 and Celite, and the filtrate was concentrated. The obtained residue was purified by silica gel column chromatography (EtOAc:hexane=70:30 to 100:0), and then purified by basic silica gel column chromatography (EtOAc/hexane) to obtain 3-{4-[3-({[tert-butyl(dimethyl)silyl]oxy}methyl)-2-fluorophenyl]piperazin-1-yl}pyridazine (325 mg).

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationfiltered by the addition of CHCl3 and Celite
3. concentrationthe filtrate was concentrated
4. customThe obtained residue was purified by silica gel column chromatography (EtOAc:hexane=70:30 to 100:0)
5. custompurified by basic silica gel column chromatography (EtOAc/hexane)