反应详情

In 10 ml of benzene, were dissolved 683 mg of methyl hydroxymethoxyacetate and 1.00 g of (S)-2-(anilinomethyl)pyrrolidine. The resulting solution was refluxed for 30 minutes while removing the water by azeotropic distillation. On removing the solvent by distillation in vacuo, there were obtained 1.38 g of 2-carbomethoxy-3-phenyl-1,3-diazabicyclo[3,3,0]octane, a derivative of glyoxylic acid. NMR peaks: δ(ppm)=1.5-2.3 (4H, multiplet), 2.3-4.1 (5H, multiplet), 3.5 (3H, singlet), 4.6 (1H, singlet), 6.2-7.1 (5H, multiplet). After having been purified by alumina column chromatography and short-path distillation, the substance showed the following results of elementary analysis:

1. temperatureThe resulting solution was refluxed for 30 minutes
2. customwhile removing the water
3. distillationby azeotropic distillation
4. customOn removing the solvent
5. distillationby distillation in vacuo