反应详情

2-{(1S,2S)-2-[1-(5-chloropyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethanamine (30 mg, 0.11 mmol) from Example 5 step 3 was dissolved in NMP (0.21 mL), DBU (24.4 mg, 0.16 mmol) was added, stirred at room temperature for 5 minutes. 1-fluoro-4-(methylsulfonyl)benzene (22.3 mg, 0.13 mmol) was added. Reaction was heated to 110° C. for 17 hours. The reaction was cooled down to room temperature, water (10 mL) was added, extracted with EtOAc (10 mL×2), second wash with Brine (10 mL). The organic phase was dried by magnesium sulfate, filter, concentrated and purified by purified by column chromatography through a 12 gram RediSep Rf™ silica gel cartridge eluting with 30% acetone/hexanes to give the title compound as a white solid.

1. customReaction
2. temperaturewas heated to 110° C. for 17 hours
3. temperatureThe reaction was cooled down to room temperature
4. extractionextracted with EtOAc (10 mL×2)
5. washsecond wash with Brine (10 mL)
6. dry with materialThe organic phase was dried by magnesium sulfate
7. filtrationfilter
8. concentrationconcentrated
9. custompurified
10. customby purified by column chromatography through a 12 gram RediSep Rf™ silica gel cartridge
11. washeluting with 30% acetone/hexanes