Reacción #2833

ord-7cc7d41500194b2d804cca39c54e96aa

Ecuación de reacción

O=C(c1cccc([N+](=O)[O-])c1)N1CCOCC1
compound ( [13]-(132)-158 )
O=C(c1cccc([N+](=O)[O-])c1)N1CCOCC1
3-nitrobenzoic acid morpholide
Nc1cccc(C(=O)N2CCOCC2)c1
compound ( [13]-(133)-158 )
Rendimiento 100.5%
Nc1cccc(C(=O)N2CCOCC2)c1
3-aminobenzoic acid morpholide
Rendimiento 100.5%

Condiciones de reacción

Temperatura
50°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrothe catalyst was removed by filtration through celite
  2. 2
    ConcentraciónThe solution was concentrated
  3. 3
    Otrothe residue was purified by silica gel column chromatography (Kieselgel 60=120 g, ethyl acetate)

Procedimiento

The compound ([13]-(132)-158) (8.63 g) prepared in Example 83 was dissolved in ethanol (400 ml), and the solution was heated to 50° C. To the suspention, a solution of 10% Pd/C (2.25 g) in ethanol and hydrazine monohydrate (4.4 ml) were added to the solution. The mixture was stirred for 30 minutes. After the reaction was completed, the catalyst was removed by filtration through celite. The solution was concentrated, and the residue was purified by silica gel column chromatography (Kieselgel 60=120 g, ethyl acetate) to obtain the above-captioned compound ([13]-(133)-158) (7.57 g) as a white solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05731310uspto-grants-1998_03