Reaction #3316979
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US03970698
Conditions: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: Diethyl diglycolate is prepared by slurrying 270 parts sodium hydride in 2800 parts tetrahydrofuran and adding 705 parts ethyl glycolate to the mixture while maintaining the temperature between 10° to 15°C. The mixture is stirred for 1 hour at 25°C, cooled to 15°C and 894 parts ethyl bromoacetate is added. The mixture is stirred for 12 hours at 25°C; solvent evaporated; residue washed with water to remove salts; dried and purified diethyl digylcolate recovered by distillation under reduced pressure. (Note: Diethyl methylglycolate or diethyl ethyldiglycolate are prepared by similar procedures wherein ethyl lactate (800 parts) or ethyl-2-hydroxybutyrate (895 parts) are, respectively, substituted for the ethyl glycolate.) while maintaining the temperature between 10° to 15°C cooled to 15°C The mixture is stirred for 12 hours at 25°C solvent evaporated residue washed with water to remove salts dried purified diethyl digylcolate recovered by distillation under reduced pressure
Source ID: ord-0e8b887365f344dda23124b10a8d5c72