反应详情

A mixture of 1.5 g (4.1 mmol) of 2-chloromethyl-1-methylbenzimidazol-5-yl-carboxylic acid-N-(n-propyl)-N-(2-ethoxycarbonylethyl)amide and 0.65 g (4.8 mmol) of p-cyanothiophenol was heated in 10 mL of dimethylformamide and 10 mL of diisopropylethylamine for 1 hour to 100° C. The solvent was distilled off in vacuo, the crude product was dissolved in 30 mL ethyl acetate, washed with 30 mL water, and after concentration purified by flash chromatography (silica gel; methylene chloride/ethanol (49:1 to 19:1). Yield: 1.5 g (79% of theory) of brown oil; Rf value: 0.65 (silica gel; ethyl acetate/ethanol/ammonia=90:10:1).

1. distillationThe solvent was distilled off in vacuo
2. dissolutionthe crude product was dissolved in 30 mL ethyl acetate
3. washwashed with 30 mL water
4. concentrationafter concentration
5. custompurified by flash chromatography (silica gel