Reaktion #652990

Reaktionsgleichung

potassium tert-butylate

2,6-dimethoxyacetophenone

ethyl oxalate

→

expected product

Ethyl 4-(2,6-dimethoxyphenyl)-4-oxido-2-oxo-3-butenoate potassium salt

Lösungsmittel

ethanol

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture is heated
2. 2
   Temperaturto reflux
3. 3
   Temperaturrefluxing
4. 4
   workup.DISTILLATION40 ml of ethanol are then distilled off
5. 5
   Temperaturto cool
6. 6
   workup.STIRRINGwith stirring for two and a half hours
7. 7
   FiltrationThe mixture is filtered
8. 8
   Waschenthe precipitate is washed with 40 ml of ethanol
9. 9
   Sonstigedried under vacuum at 60° C. for 17 hours

Vorschrift

A solution of 13.4 g of 95% potassium tert-butylate in 72 ml of ethanol is added over 6 minutes to a solution, stirred and heated to 50° C., of 18 g of 2,6-dimethoxyacetophenone in 54 ml of ethanol. The mixture is heated to reflux, 16.3 ml of ethyl oxalate are added over 9 minutes and refluxing is continued for 1 hour. 40 ml of ethanol are then distilled off and the mixture is allowed to cool with stirring for two and a half hours. The mixture is filtered, and the precipitate is washed with 40 ml of ethanol and dried under vacuum at 60° C. for 17 hours to obtain 31 g of expected product.

Quelle