反应详情

温度

0 °C

To 50 ml of anhydrous ethanol stirred at 0°-5° C., 2 ml thionyl chloride were added. At the same temperature 2.1 g (0.01 mol) of sodium 2-(1-methylethyl)-5-oxo-1imidazolidineacetate were added. The suspension obtained was stirred at 0° C. for 1 hour and at room temperature for 2 hours. The solvent was evaporated under reduced pressure and the residue taken up with ethyl acetate. The solid residue was filtered off and the solvent evaporated. The residue was dissolved in a saturated solution of sodium hydrogen carbonate and extracted with 3×50 ml of dichloromethane. The organic layers were dried and evaporated to give ethyl 2-(1-methylethyl)-5-oxo-1imidazolidineacetate (0.9 g) as a pale-yellow oil (42%) (Rf 0.6, ethyl acetate/dichloromethane 6:4; silica gel plates). Hydrochloride salt, m.p. 148°-149° C. (methanol/ethyl acetate).

1. customThe suspension obtained
2. customThe solvent was evaporated under reduced pressure
3. filtrationThe solid residue was filtered off
4. customthe solvent evaporated
5. dissolutionThe residue was dissolved in a saturated solution of sodium hydrogen carbonate
6. extractionextracted with 3×50 ml of dichloromethane
7. customThe organic layers were dried
8. customevaporated