反应详情

温度

130 °C

A mixture of 3-[4-(2-bromo-5-fluorophenoxy)piperidin-1-yl]isoxazole-5-carbonitrile (1.4 g, 3.82 mmol), pyridinium hydrochloride (0.9 g, 7.79 mmol) and sodium azide (1.3 g, 20.00 mmol) in NMP (12 mL) was stirred and heated at 130° C. bath for 2 h. After cooling, the mixture was diluted with water and acidified with 1N HCl (some precipitate appeared). The whole mixture was then extracted with EtOAc. The EtOAc extract was washed with water (3×), dried (Na2SO4) and concentrated. The residue was triturated with diethyl ether to give the title compound as a light brown powder.

1. temperatureAfter cooling
2. extractionThe whole mixture was then extracted with EtOAc
3. extractionThe EtOAc extract
4. washwas washed with water (3×)
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customThe residue was triturated with diethyl ether