反应详情

温度

80 °C

A stirred solution of 2-[4-(hydroxymethyl)phenyl]-1,3-oxazole-4-carboxylic acid (0.99 g, 4.5 mmol) in DMF was treated sequentially with EDC (1.04 g, 5.4 mmol), HOBt (0.67 g, 5.0 mmol and pyrrolidine (0.35 g, 5.0 mmol), stirred at 80° C. for 4 hours and evaporated to dryness. The resultant residue was dissolved in EtOAc and water. The layers were separated and the organic layer was washed successively with 1M HCl, water, saturated NaHCO3 and brine, dried over Na2SO4 and concentrated under reduced pressure The resultant residue was purified by flash chromatography (silica, EtOAc:hexanes 25%) to give the title product in 84% yield, identified by NMR and mass spectral analyses. LCMS (ESI+) 273 (MH+).

1. customevaporated to dryness
2. dissolutionThe resultant residue was dissolved in EtOAc
3. customThe layers were separated
4. washthe organic layer was washed successively with 1M HCl, water, saturated NaHCO3 and brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated under reduced pressure The resultant residue
7. customwas purified by flash chromatography (silica, EtOAc:hexanes 25%)