反应详情

To 7.64 g (0.025 mole) of the ethyl 3-acetoxy-2,4,5-trifluorobenzoylacetate (VIII) thus obtained were added 20 ml of acetic anhydride and 6 ml of ortho-ethyl formate and the mixture was refluxed for 2 hours and then condensed under reduced pressure. The residue was dissolved in 50 ml of dichloromethane, added 1.91 g (0.026 mole) of DL-2-aminopropanol and allowed to stand over night. Dichloromethane was distilled under reduced pressure and the residue was applied to silica gel column chromatography (solvent: mixture of toluene:ethyl acetate=1:1) to give 4.37 g of the ethyl-2-(3-acetoxy-2,4,5-trifluorobenzoyl)-3-(2-hydroxy-1-methylethyl)aminoacrylate (X) as pale yellow oily product. ##STR10##

1. temperaturethe mixture was refluxed for 2 hours
2. customcondensed under reduced pressure
3. waitto stand over night
4. distillationDichloromethane was distilled under reduced pressure
5. additionthe residue was applied to silica gel column chromatography (solvent: mixture of toluene:ethyl acetate=1:1)