反应详情

温度

0 °C

To a stirred solution of 3-(2,2,2-trichloroethyloxycarbonylamino)isoxazole (1.30 g, 5.0 mmol), 5(R)-hydroxymethyl-3-(3-fluoro-4-(1-benzyl-1,2,5,6-tetrahydropyrid-4-yl)phenyl)oxazolidin-2-one (WO 97/30995; 1.91 g, 5.0 mmol) and tributylphosphine (1.52 g, 7.5 mmol) in dry tetrahydrofuran (50 ml) under a nitrogen atmosphere at 0° C., was added 1,1′-(azodicarbonyl)dipiperidine (1.89 g, 7.5 mmol) in dry tetrahydrofuran (15 ml). The solution was stirred at 0° C. for 30 minutes before being allowed to come to room temperature and it was then stirred for 2 days. The mixture was filtered, concentrated by rotary evaporation and chromatographed by MPLC (30% ethyl acetate/hexane, ICN Alumina N 32–63), and triturated with ether to give the title compound as a white amorphous solid (1.62 g, 52%).

1. customto come to room temperature
2. stirringit was then stirred for 2 days
3. filtrationThe mixture was filtered
4. concentrationconcentrated by rotary evaporation
5. customchromatographed by MPLC (30% ethyl acetate/hexane, ICN Alumina N 32–63)
6. customtriturated with ether