HRID1392079

反应详情

EQUATION

反应方程式

HRID 1392079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. filtrationThe reaction mixture was filtered through Celite
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue was dissolved in DCM
  4. washwashed with saturated NaHCO3, brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated to a viscous oil
  8. extractionThe aqueous layer was extracted with DCM (3×)
  9. washThe combined organic layer was washed with brine
  10. dry with materialdried (Na2SO4)
  11. filtrationfiltered
  12. concentrationconcentrated to a viscous oil