反应详情

温度

160 °C

In a pressure reaction tube was added 5-chloropyrazolo[1,5-a]pyrimidine (4.2 g, 27 mmol), (R)-2-(2,5-difluorophenyl)pyrrolidine (Preparation A; 5.3 g, 29 mmol), anhydrous n-butanol (5 ml, 55 mmol), and DIEA (9.5 ml, 55 mmol). The yellowish suspension was sealed and heated in an oil bath (160° C.) overnight. The reaction was cooled to ambient temperature, diluted with EtOAc (250 mL), and filtered, rinsing the solid with EtOAc. The filtrate (330 mL) was washed with water (2×150 mL), brine (100 mL), concentrated, and purified by silica chromatography, eluting with 2:1 EtOAc/hexanes to give the product as a bright yellowish solid (5.6 g, 68% yield).

1. customIn a pressure reaction tube
2. customPreparation A
3. customThe yellowish suspension was sealed
4. temperatureThe reaction was cooled to ambient temperature
5. filtrationfiltered
6. washrinsing the solid with EtOAc
7. washThe filtrate (330 mL) was washed with water (2×150 mL), brine (100 mL)
8. concentrationconcentrated
9. custompurified by silica chromatography
10. washeluting with 2:1 EtOAc/hexanes