反应详情

The compound obtained in step (a) (0.050 g, 0.15 mmol) was dissolved in EtOAc (15 ml) under magnetic stirring. To this solution was added N-hydroxyacetimidoyl chloride (0.15 g, 1.6 mmol), water (0.3 ml) and KHCO3 (0.16 g, 1.6 mmol). The mixture was stirred for 2 days at which time LC-MS showed 90% conversion. The reaction was stopped and the mixture was partitioned between EtOAc (25 ml) and water (25 ml). The organic phase was washed (water, brine) and dried. Filtration and evaporation gave a crude mixture which was purified by chromatography on silica. Freeze-drying the pure fractions afforded the subtitle compound (0.031 g, 53%) as a white powder.

1. customthe mixture was partitioned between EtOAc (25 ml) and water (25 ml)
2. washThe organic phase was washed (water, brine)
3. customdried
4. filtrationFiltration and evaporation
5. customgave a crude mixture which
6. customwas purified by chromatography on silica
7. customFreeze-drying the pure fractions