HRID1392079
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
A mixture of benzyl [(3R,7S)-1-methyl-2-oxo-7-phenyl-2,3,4,7-tetrahydro-1H-azepin-3-yl]carbamate (3c) (310 mg) and Pearlman's catalyst (62 mg) in EtOH (8 mL) was hydrogenated at 45 psi for 6 h. The reaction mixture was filtered through Celite and concentrated in vacuo. The residue was dissolved in DCM and washed with saturated NaHCO3, brine, dried (Na2SO4), filtered and concentrated to a viscous oil. The aqueous layer was extracted with DCM (3×). The combined organic layer was washed with brine, dried (Na2SO4), filtered and concentrated to a viscous oil. (166 mg, 86%).
WORKUP
后处理
- filtrationThe reaction mixture was filtered through Celite
- concentrationconcentrated in vacuo
- dissolutionThe residue was dissolved in DCM
- washwashed with saturated NaHCO3, brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated to a viscous oil
- extractionThe aqueous layer was extracted with DCM (3×)
- washThe combined organic layer was washed with brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated to a viscous oil