2-甲氧基乙烷酰亚胺

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-methoxy-acetamidine (7.21 g, 89.19 mmol) in EtOH (50 ml) was added sodium ethylate (26 ml, 22% solution in EtOH) and the reaction mixture was heated to 50° C. for 30 min. A solution of mucobromic acid (6.5 g, 38.77 mmol) in EtOH (50 ml) was added followed by sodium ethylate (14 ml, 22% solution in EtOH), and the reaction mixture was continued to stir at 50° C. for 1 h. After filtration and solvent evaporation, water (5 ml) was added, the reaction mixture was cooled to 0° C. and acidified with 2N HCl solution to pH ˜6. After evaporation of water, the residue was dissolved in MeOH, filtered, and the filtrate was evaporated. The crude material was purified by silica gel chromatography using a methanol/methylenechloride eluent as solvent to yield 3.73 g (60%) of the title compound. After filtration and solvent evaporation, water (5 ml) was added the reaction mixture was cooled to 0° C. After evaporation of water the residue was dissolved in MeOH filtered the filtrate was evaporated The crude material was purified by silica gel chromatography