Реакция #2833

ord-7cc7d41500194b2d804cca39c54e96aa

Растворители

Условия реакции

Температура
50°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05731310uspto-grants-1998_03