Reacción #569915

ord-cfbd7a20e5c54dc2993cf61bbe163d96

Ecuación de reacción

CCOCC
ether
[N-]=[N+]=NC1CCc2ccccc2NC1=O
3-azido-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one
CCO
ethanol
NC1CCc2ccccc2NC1=O
3-amino-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONwas added
  2. 2
    workup.ADDITIONwas added
  3. 3
    Filtraciónthe catalyst was filtered off
  4. 4
    Otrothe solvent removed under reduced pressure
  5. 5
    Otroto give an oil which

Procedimiento

To a solution of 3-azido-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one (see Example 1) (27 g) in 2B ethanol (3500 ml) stirring at room temperature under an atmosphere of nitrogen, a suspension of Raney nickel in water (50 ml, washed with 10 volumes of ethanol) was added. The mixture was stirred at room temperature for 2 hours when an additional 30 ml of Raney nickel suspension was added. After stirring for an additional 30 minutes, the catalyst was filtered off and the solvent removed under reduced pressure to give an oil which solidified on addition of ether to give 3-amino-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one, melting at 161°-2°.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04575503uspto-grants-1986_03