反応 #652990

反応方程式

potassium tert-butylate

2,6-dimethoxyacetophenone

ethyl oxalate

→

expected product

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

溶媒

ethanol

ethanol

反応条件

後処理

1. 1
   温度The mixture is heated
2. 2
   温度to reflux
3. 3
   温度refluxing
4. 4
   workup.DISTILLATION40 ml of ethanol are then distilled off
5. 5
   温度to cool
6. 6
   workup.STIRRINGwith stirring for two and a half hours
7. 7
   ろ過The mixture is filtered
8. 8
   洗浄the precipitate is washed with 40 ml of ethanol
9. 9
   その他dried under vacuum at 60° C. for 17 hours

実験手順

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.

出典