反应详情

To a stirred solution of 1-({1-[(6-methylpyridin-3-yl)carbonyl]azetidin-3-yl}carbonyl)-1,4-diazepane (60 mg, 0.194 mmol) in EtOH (3 mL) was added Pd/C (10% wt/wt, 6 mg) and acetone (143 μL, 1.95 mmol). The flask was purged with N2 (N2/vacuum cycle×3) and then H2 (H2/vacuum cycle×3). After 24 hours the reaction was filtered through Celite® and concentrated at reduced pressure. Purification by silica FCC (90:9:1 Et2O/MeOH/NH3) and capture and release (SCX-2, flush with MeOH, then release with 7M NH3 in MeOH) gave the title compound (18.4 mg, 27%).

1. customThe flask was purged with N2 (N2/vacuum cycle×3)
2. filtrationAfter 24 hours the reaction was filtered through Celite®
3. concentrationconcentrated at reduced pressure
4. customPurification by silica FCC (90:9:1 Et2O/MeOH/NH3) and capture and release (SCX-2,
5. customflush with MeOH