反应详情

A stirred solution of tert-butyl 4-({1-[(benzyloxy)carbonyl]azetidin-3-yl}carbonyl)-1,4-diazepane-1-carboxylate (1.54 g, 3.69 mmol) in EtOH (10 mL) was purged with N2 and charged with 10% Pd/C (154 mg, 10% wt/wt). The flask was purged with N2 (N2/vacuum cycle×3) and then H2 (H2/vacuum cycle×3). After 24 hours the reaction was incomplete by NMR analysis. The mixture was filtered through Celite®, fresh catalyst charged (154 mg, 10% wt/wt) and the hydrogenation resumed and after a further 24 and 48 hours this process was repeated. NMR analysis confirmed consumption of starting material and the reaction was filtered through Celite® and concentrated at reduced pressure to give the title compound (1.02 g, 98%).

1. customThe flask was purged with N2 (N2/vacuum cycle×3)
2. filtrationThe mixture was filtered through Celite®, fresh catalyst
3. additioncharged (154 mg, 10% wt/wt)
4. customafter a further 24 and 48 hours
5. customconsumption of starting material
6. filtrationthe reaction was filtered through Celite®
7. concentrationconcentrated at reduced pressure