HRID1402730
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of benzyl 3-[(4-cyclobutyl-1,4-diazepan-1-yl)carbonyl]azetidine-1-carboxylate (420 mg, 1.13 mmol) in EtOH (10 ml) was added 5% Pd—C (42 mg, 10% wt/wt). The flask was evacuated and the vacuum purged with N2 gas. The flask was evacuated again and the vacuum purged with H2 gas. The reaction was complete after 16 h, as shown by 1H NMR. The suspension was filtered through Celite® with MeOH washings (3×5 ml), and the combined filtrate dried (MgSO4), filtered and concentrated at reduced pressure to give the title compound (248 mg, 93% yield) as a viscous pale yellow oil.
WORKUP
后处理
- customThe flask was evacuated
- customthe vacuum purged with N2 gas
- customThe flask was evacuated again
- customthe vacuum purged with H2 gas
- filtrationThe suspension was filtered through Celite® with MeOH washings (3×5 ml)
- dry with materialthe combined filtrate dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated at reduced pressure