反应详情

To a stirred solution of 1-(azetidin-3-ylcarbonyl)-4-cyclobutylpiperazine (60 mg, 0.27 mmol) in dichloromethane (1 mL) at 0° C., was added 6-methylpyridine-3-carbonyl chloride (31 mg, 0.32 mmol) and DIPEA (142 μL, 0.81 mmol). After 4 hours the reaction was quenched by addition of saturated aq. NaHCO3 (1 mL) and the aqueous extracted with dichloromethane (2×5 mL), dried (MgSO4), filtered, and concentrated at reduced pressure. Purification by silica FCC (eluting with 90:9:1 Et2O/MeOH/NH3) followed by capture and release on an SCX-2 cartridge (washing with MeOH and releasing with 7M NH3 in MeOH) gave the title compound (17.8 mg, 19%)

1. customAfter 4 hours the reaction was quenched by addition of saturated aq. NaHCO3 (1 mL)
2. extractionthe aqueous extracted with dichloromethane (2×5 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated at reduced pressure
6. customPurification
7. washby silica FCC (eluting with 90:9:1 Et2O/MeOH/NH3)
8. washfollowed by capture and release on an SCX-2 cartridge (washing with MeOH and releasing with 7M NH3 in MeOH)