反应详情

温度

100 °C

2-{(1S,2R)-2-[1-(5-chloropyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethyl 4-methylbenzenesulfonate (65 mg, 0.15 mmol) from step 1 of this example was dissolved in dioxane (1.2mL). Sodium azide (22.3 mg, 0.34 mmol) was added, then water (0.3 mL). The reaction was heated to 100° C. to reflux for 2 hours. The reaction was cooled to room temperature, water (10 mL) was added and extracted with EtOAc (10 mL×2). The combined organic phase was dried by magnesium sulfate, filter, concentrated and purified by column chromatography through a 12 gram RediSep Rf™ silica gel cartridge eluting with 5% ethyl acetate/hexanes to give the title compound as a white solid.

1. temperatureto reflux for 2 hours
2. temperatureThe reaction was cooled to room temperature
3. extractionextracted with EtOAc (10 mL×2)
4. dry with materialThe combined organic phase was dried by magnesium sulfate
5. filtrationfilter
6. concentrationconcentrated
7. custompurified by column chromatography through a 12 gram RediSep Rf™ silica gel cartridge
8. washeluting with 5% ethyl acetate/hexanes