反应详情

温度

140 °C

A suspension of 6-chloro-3-nitroimidazo[1,2-b]pyridazine (1.0 g, 5.0 mmol) and (R)-2-(2,5-difluorophenyl)pyrrolidine (Prepared as described in Preparation A; 1.9 g, 11 mmol) in n-butanol (4.6 mL, 50 mmol) was sealed in a pressure reaction tube and stirred in a 140° C. oil bath overnight. After cooling to ambient temperature, the reaction mixture was diluted with EtOAc (250 mL), then washed with water (2×150 mL) and brine (150 mL), filtered through a Biotage Phase Separator filter paper and concentrated. The crude material was purified by silica gel chromatography, eluting with 2:1 EtOAc/hexanes to yield the product as a foamy yellow powder (1.3 g, 75% yield).

1. customwas sealed in a pressure reaction tube
2. temperatureAfter cooling to ambient temperature
3. washwashed with water (2×150 mL) and brine (150 mL)
4. filtrationfiltered through a Biotage Phase Separator
5. filtrationfilter paper
6. concentrationconcentrated
7. customThe crude material was purified by silica gel chromatography
8. washeluting with 2:1 EtOAc/hexanes