反应详情

A stirred mixture (5R)-3-{6-[4-(3-bromophenyl)butoxy]hexyl}-5-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)-1,3-oxazolidin-2-one (1.0 g), N-methylethenesulphonamide (WO 95/09166), (462 mg), tri-o-tolylphosphine (200 mg), palladium acetate (165 mg) and triethylamine (5 ml) in dry DMF (15 ml) was heated at 90° C. for 18 h. The mixture was cooled and filtered. The filtrate was poured into water (200 ml) and extracted into ethyl acetate (3×50 ml). The combined extracts were washed with water (100 ml) and (Na2SO4) and evaporated in vacuo. The residual oil was purified by chromatography on Biotage (40 g) eluting with diethyl ether-ethyl acetate (9:1) to give the title compound (220 mg). LCMS RT=3.70 min.

1. temperatureThe mixture was cooled
2. filtrationfiltered
3. additionThe filtrate was poured into water (200 ml)
4. extractionextracted into ethyl acetate (3×50 ml)
5. washThe combined extracts were washed with water (100 ml) and (Na2SO4)
6. customevaporated in vacuo
7. customThe residual oil was purified by chromatography on Biotage (40 g)
8. washeluting with diethyl ether-ethyl acetate (9:1)