ethyl 2-[2-(2-ethoxy-2-oxoethoxy)ethoxy]acetate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The mixing was carried out under a protective nitrogen gas atmosphere. 7.93 g (80.0 mmol) sodium-tert-butoxide were placed in 150 ml THF and heated to boiling point. At this temperature 8.50 g (36.3 mmol) ethyl (2-ethoxycarbonylmethoxy-ethoxy)-acetate (prepared analogously to Canadian Journal of Chemistry; 74; 8; 1996; 1437-1446) in 100 ml THF were added dropwise within 3 h. After the addition had ended the mixture was refluxed for 1 h and then stirred overnight at RT. Then the reaction mixture was adjusted to pH 5 with glacial acetic acid and concentrated by rotary evaporation. The residue was mixed with water and extracted with ethyl acetate. The organic phases were combined, dried and the solvent was eliminated under reduced pressure and with gentle heating. heated After the addition was refluxed for 1 h concentrated by rotary evaporation The residue was mixed with water extracted with ethyl acetate dried