Reaktion #41954
ord-fc9b9235d9cf49359251140b795631d9
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturby refluxing
- 2FiltrationAfter filtration
- 3Extraktionthe filtrate was extracted with ethyl acetate (500 mL)
- 4EinengenThe organic layer was subjected to vacuum concentration
- 5workup.DISTILLATIONto vacuum distillation at 132-135° C.
Vorschrift
Chloroacetaldehyde dimethyl acetal (50.0 g), potassium benzoate (70.7 g), potassium iodide (6.66 g) and DMF (N,N-dimethylformamide) (250 mL) were placed in a three-neck flask, followed by refluxing. Twenty hours later, the reaction mixture was cooled to room temperature, and water (250 mL) and ethyl acetate (250 mL) were added thereto, followed by stirring. After filtration, the filtrate was extracted with ethyl acetate (500 mL). The organic layer was subjected to vacuum concentration and then to vacuum distillation at 132-135° C. and at 5 mmHg and thereby yielded the target compound (61.0 g) in a yield of 72%.