Reaktion #83765
ord-73f060dfe6de4044aca39bfe30d68e8e
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.DISTILLATIONAt the end of this time, the reaction mixture was freed from dimethylformamide by distillation under reduced pressure
- 2SonstigeThe residue thus obtained
- 3Extraktionafter which it was extracted with ethyl acetate
- 4WaschenThe extract was washed with water
- 5Trocknendried over anhydrous sodium sulfate
- 6Sonstigeafter which the solvent was removed by distillation under reduced pressure
- 7SonstigeThe resulting residue was crystallized by trituration with hexane
Vorschrift
A solution of 56 g of 4-nitrophenol, 90 g of methyl bromoacetate and 100 g of potassium carbonate in 500 ml of dimethylformamide was stirred at room temperature for 2 days. At the end of this time, the reaction mixture was freed from dimethylformamide by distillation under reduced pressure. The residue thus obtained was diluted with water, after which it was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous sodium sulfate, after which the solvent was removed by distillation under reduced pressure. The resulting residue was crystallized by trituration with hexane, to give 63.3 g of the title compound, melting at 98°-99° C.