反应详情

温度

110 °C

To a solution of 2-(pyrrol-1-yl)malonic acid diethyl ester (75.7 g) in benzyl alcohol (200 ml) was added tetraethyl titanate (3.0 g), and the resulting mixture was stirred at 110° C. for 15 hours. After removal of the benzyl alcohol under reduced pressure, the residue was chromatographed on silica gel using n-hexane/ethyl acetate (10:1) as the eluent. Fractions containing the title compound were pooled and evaporated under reduced pressure. The residue was recrystallized from ethyl acetate/n-hexane to give the title compound (102.5 g, 87.3%) as colorless crystals, mp 48.5°-49° C.

1. customAfter removal of the benzyl alcohol under reduced pressure
2. customthe residue was chromatographed on silica gel
3. additionFractions containing the title compound
4. customevaporated under reduced pressure
5. customThe residue was recrystallized from ethyl acetate/n-hexane