反应详情

A suspension of 15.5 g (0.05 mol) of 2-(4-acetamidobutyryl)-5-chlorohydrocinnamic acid and 8.50 g (0.052 mol) of 1,1'-carbonyldiimidazole in 350 ml of tetrahydrofuran is stirred at room temperature for 2 hours and 4.00 g (0.052 mol) of glycolamide are added thereto. After stirring at room temperature overnight, the solution is concentrated, extracted with methylene chloride/water, dried with magnesium sulfate and the solvent is distilled in a vacuum. Chromatography on silica gel with methylene chloride-methanol (20:1) and crystallization from ethyl acetate/ether gives carbamoylmethyl 2-(4-acetamidobutyryl)-5-chlorohydrocinnamate as white crystals with melting point 114°-116°.

1. stirringAfter stirring at room temperature overnight
2. concentrationthe solution is concentrated
3. extractionextracted with methylene chloride/water
4. dry with materialdried with magnesium sulfate
5. distillationthe solvent is distilled in a vacuum
6. customChromatography on silica gel with methylene chloride-methanol (20:1) and crystallization from ethyl acetate/ether