2-(甲氨基)-乙醛缩二乙醇

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of methyl 5-[2-(2-[2,2,2-trifluoroethyl]guanidino)pyrid-6-ylthio]valerimidate (0.3 g.) and N-methyl-2,2-diethoxyethylamine (0.44 g.) in MeOH (3 ml.) was kept at room temperature for 48 hours and then evaporated to dryness. The residue was dissolved in concentrated aqueous HCl and the solution heated at 90° for 30 minutes and then evaporated to dryness. The residue was partitioned between H2O and EtOAc and the aqueous phase basified with 10N NaOH and then extracted with EtOAc. The EtOAc extract was dried and evaporated to dryness and the residue dissolved in acetone. This solution was added to a solution of maleic acid in acetone, and the precipitate (0.12 g.) was collected and crystallised from EtOH to give 1-methyl-2-[4-(2-[2-(2,2,2-trifluoroethyl)guanidino]pyrid-6-ylthio)butyl]imidazole hydrogen maleate, m.p. 107°-110°. evaporated to dryness The residue was dissolved in concentrated aqueous HCl the solution heated at 90° for 30 minutes evaporated to dryness The residue was partitioned between H2O and EtOAc extracted with EtOAc The EtOAc extract was dried evaporated to dryness the residue dissolved in acetone This solution was added to a solution of maleic acid in acetone the precipitate (0.12 g.) was collected crystallised from EtOH