反应详情

温度

60 °C

A suspension of (S)-glycidyl nosylate (0.29 g), caesium carbonate (1.82 g) and N-(1-adamantylmethyl)-5-bromo-2hydroxyisonicotinamide (0.41 g) (Example 35(ii)) in anhydrous N,N-dimethylformamide (6 ml) was heated at 60° C. under nitrogen for 2 hours. The reaction mixture was allowed to cool to room temperature, diluted with water (50 ml) and extracted into ethyl acetate (3×20 ml). The combined extracts were dried over anhydrous sodium sulphate, filtered and concentrated. The residue was purified by chromatography on silica gel eluting with dichloromethane:ethyl acetate (4:1 to 0:1) to afford the sub-titled compound (0.12 g).

1. temperatureto cool to room temperature
2. extractionextracted into ethyl acetate (3×20 ml)
3. dry with materialThe combined extracts were dried over anhydrous sodium sulphate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by chromatography on silica gel eluting with dichloromethane:ethyl acetate (4:1 to 0:1)