反应详情

温度

80 °C

N-(2-{(1S,2S)-2-[1-(5-chloropyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethyl)-N-[4-(4H-1,2,4-triazol-4-yl)phenyl]acetamide from step 1 of this example was dissolved in ethanol (0.5 mL), added sodium hydroxide (60% w/w, 0.3 mL) and heated to 80° C. for 5.5 hours. The reaction was cooled to room temperature, water (10 mL) was added and extracted with ethyl acetate (20 mL). The organic phase was dried by magnesium sulfate, filtered, concentrated and purified by column chromatography through a 25 gram Biotage SNAP KP-Sil™ silica gel cartridge eluting with 50% acetone/hexanes to give the title compound as a white-solid.

1. temperatureThe reaction was cooled to room temperature
2. extractionextracted with ethyl acetate (20 mL)
3. dry with materialThe organic phase was dried by magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. custompurified by column chromatography through a 25 gram Biotage SNAP KP-Sil™ silica gel cartridge
7. washeluting with 50% acetone/hexanes