反应详情

To a stirred solution of 1-[(4-cyclobutyl-1,4-diazepan-1-yl)carbonyl]azetidin-3-ol (40 mg, 0.158 mmol) in DMSO (2 ml) was added NaH (14 mg, 0.316 mmol, 60 in mineral oil) at RT in one portion. The suspension was stirred for 2 h at RT then 6-chloro-N-methylpyridine-3-carboxamide (54 mg, 0.316 mmol) was added in one portion. The mixture was heated at 80-100° C. in a sealed tube over night. After cooling to RT, the solution was partitioned between brine/water (1:1 mixture, 15 ml) and DCM (20 ml). The organic layer was separated, washed with brine (2×20 ml), dried (Na2SO4), filtered and concentrated at reduced pressure. The residue was purified by preparative HPLC to provide the title compound as white solid (83 mg, 56% yield).

1. temperatureThe mixture was heated at 80-100° C. in a sealed tube over night
2. temperatureAfter cooling to RT
3. customthe solution was partitioned between brine/water (1:1 mixture, 15 ml) and DCM (20 ml)
4. customThe organic layer was separated
5. washwashed with brine (2×20 ml)
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated at reduced pressure
9. customThe residue was purified by preparative HPLC