反应详情

A flask containing a solution of the Cbz-protected amine 11b (460 mg, 0.846 mmol) in a 5:1 MeOH/EtOAc mixture (12 mL) was purged and filled 3 times with argon, then 10% Pd/C (50 mg) was added. The flask was purged and filled 3 times with H2, and the resulting black suspension was stirred at rt under H2 (1 atm). Since the reaction did not reach completion after 3 h, an additional amount of 10% Pd/C (30 mg) was added and stirring under H2 was continued for 5 h. The reaction mixture was then filtered through a pad of Celite, the Celite washed with MeOH and AcOEt, and the solution concentrated in vacuo to yield 317 mg (92%) of the crude title compound as a pale yellow oil, that was used for the next step without further purification.

1. customwas purged
2. additionfilled 3 times with argon
3. addition10% Pd/C (50 mg) was added
4. customThe flask was purged
5. additionfilled 3 times with H2
6. customafter 3 h
7. additionan additional amount of 10% Pd/C (30 mg) was added
8. stirringstirring under H2
9. filtrationThe reaction mixture was then filtered through a pad of Celite
10. washthe Celite washed with MeOH and AcOEt
11. concentrationthe solution concentrated in vacuo