反应详情

温度

50 °C

To a solution of N-(2-t-butoxycarbonylaminophenyl)-4-(2-chloropyrimidin-5-yl)benzamide (Method 53, 80 mg, 0.19 mmol) in N,N-dimethylacetamide (3.5 ml) was added 3-aminopropylpiperidine (108 mg 0.76 mmol). The reaction mixture was stirred at 50° C. for 20 hours, before being allowed to cool. The reaction mixture was partitioned between water and ethyl acetate, before being filtered under gravity, through a Varian Chem Elut (CE1010) diatomaceous earth column. The resulting solution was then concentrated under reduced pressure and purified by flash column chromatography, eluting with methanol/dichloromethane (0-20%), to give the title compound, which was used without further purification; Mass Spectrum: M+H+ 531.

1. temperatureto cool
2. customThe reaction mixture was partitioned between water and ethyl acetate
3. filtrationbefore being filtered under gravity, through a Varian Chem Elut (CE1010) diatomaceous earth column
4. concentrationThe resulting solution was then concentrated under reduced pressure
5. custompurified by flash column chromatography
6. washeluting with methanol/dichloromethane (0-20%)