反应详情

A solution of 1.8 g (5.9 mMol) of 3-amino-4-methylamino-benzoic acid-N-(n-propyl)-N-(2-ethoxycarbonylethyl)-amide [prepared analogously to 3-amino-4-ethylamino-benzoic acid-N-phenyl-N-(2-ethoxycarbonylethyl)-amide], 1.1 g (6.8 mMol) of N,N'-carbonyldiimidazole and 0.65 g (6.9 mMol) of chloroacetic acid in 75 ml tetrahydrofuran was stirred for 1 hour at room temperature. Then the solvent was distilled off in vacuo, and the crude product was purified by flash chromatography (silica gel; methylene chloride/ethanol=49:1). Yield: 1.7 g (77% of theory) yellow oil, Rf value: 0.58 (silica gel; ethyl acetate/ethanol/ammonia=90:10:1)

1. distillationThen the solvent was distilled off in vacuo
2. customthe crude product was purified by flash chromatography (silica gel; methylene chloride/ethanol=49:1)