反応 #347078

反応方程式

2,6-dimethoxyacetophenone

ethyl oxalate

sodium methylate

sodium

→

expected product

Methyl 4-(2,6-dimethoxyphenyl)-4-oxido-2-oxo-3-butenoate Sodium Salt

溶媒

MeOH

ether

MeOH

反応条件

後処理

1. 1
   温度The reaction mixture is heated
2. 2
   温度to reflux for 7 hours
3. 3
   workup.WAITleft

実験手順

A solution of 100 g of 2,6-dimethoxyacetophenone and 7.5 ml of ethyl oxalate in 520 ml of anhydrous MeOH is added slowly to a solution of sodium methylate prepared from 12.7 g of sodium and 285 ml of anhydrous MeOH. The reaction mixture is heated to reflux for 7 hours and left overnight at RT. It is poured into 2 liters of iso ether and left stirring for minutes. The expected product is obtained by filtration, washing with iso ether and drying under vacuum, m=120 g, m.p.=178° C.

出典