反应详情

A solution of 0.11 ml of acetic anhydride in 0.5 ml of tetrahydrofuran is added dropwise to a solution of 260 mg of 1-(4-aminophenyl)-3-n-propyl-3-azabicyclo[3.1.1]heptane-2,4-dione and 6 mg of 4-dimethylaminopyridine in 8 ml of tetrahydrofuran. After stirring at room temperature for 21/2 hours, two drops of ethanol are added to the reaction mixture and stirring is continued for a further 15 minutes. After concentration by evaporation and subsequent recrystallisation from ethyl acetate/petroleum ether, the title compound is obtained in the form of white crystals having a melting point of 138.5°-139.5°. Rf (methylene chloride/methanol/glacial acetic acid 40:5:1)=0.55.

1. additionare added to the reaction mixture
2. concentrationAfter concentration
3. customby evaporation and subsequent recrystallisation from ethyl acetate/petroleum ether