反应详情

2-{(1S,2S)-2-[1-(5-chloropyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethanamine (35 mg, 0.125 mmol) from Example 5 step 3 was dissolved in DMF (0.62 mL), cesium carbonate (203 mg, 0.62 mmol) was added, stirred at room temperature for 10 minutes. 2-bromo-5-(methylsulfonyl)pyridine (32.4 mg, 0.137 mmol) was added. Reaction was run at room temperature for 1 hour, then heated to 50° C. for 5 hours. 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 preparative-TLC (Analtech Silica Gel GF 1500 μM, 20×20 cm) using 30% acetone/hexane to give the title compound as a white solid.

1. customReaction
2. waitwas run at room temperature for 1 hour
3. temperatureheated to 50° C. for 5 hours
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 by preparative-TLC (Analtech Silica Gel GF 1500 μM, 20×20 cm)