反应详情

To a solution of 2-(pyrrol-1-yl)malonic acid ethyl (-)-menthyl ester (64.0 g) in chloroform (80 ml) was added trichloroacetyl chloride (69.0 g), and the resulting mixture was refluxed for 7 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in ethyl acetate. The solution was washed with 5% aqueous sodium carbonate solution and then with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was chromatographed on silica gel using n-hexane/ethyl acetate (50:1) as the eluent. Fractions containing the title compound were pooled and evaporated under reduced pressure to give the title compound (87.0 g, 94.9%) as a colorless oil.

1. temperaturethe resulting mixture was refluxed for 7 hours
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. dissolutionthe residue was dissolved in ethyl acetate
4. washThe solution was washed with 5% aqueous sodium carbonate solution
5. dry with materialwith saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe residue was chromatographed on silica gel
8. additionFractions containing the title compound
9. customevaporated under reduced pressure