Réaction #2833

ord-7cc7d41500194b2d804cca39c54e96aa

Conditions de réaction

Température
50°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

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

Mode opératoire

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05731310uspto-grants-1998_03