反应详情

N-(2-{(1S,2S)-2-[1-(5-chloropyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethyl)-4-(methylsulfonyl)aniline (6 mg, 0.014 mmol) from Example 7 and paraformaldehyde were added to dichloroethane (0.2 mL), then sodium triacetoxyborohydride (10.1 mg, 0.041 mmol) was added and stirred overnight at room temperature. The reaction was quenched with sodium bicarbonate saturated solution (10 mL), extracted with EtOAc (10 mL), second wash with Brine (10 mL). The organic phase was dried by magnesium sulfate, filtered, concentrated and purified by purified by preparative-TLC (Analtech Silica Gel GF 1500 μM, 20×20 cm) using 50% ethyl acetate/hexane to give the title compound as a white solid.

1. customThe reaction was quenched with sodium bicarbonate saturated solution (10 mL)
2. extractionextracted with EtOAc (10 mL)
3. washsecond wash with Brine (10 mL)
4. dry with materialThe organic phase was dried by magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified
8. customby purified by preparative-TLC (Analtech Silica Gel GF 1500 μM, 20×20 cm)