反応 #669937

ord-c88618cf60c24253b3403b2cb4dd7a43

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

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 litres of isopropyl ether and left stirring for 15 minutes. The expected product is obtained by filtration, washing with isopropyl ether and drying under vacuum, m=120 g, m.p.=178° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05925661uspto-grants-1999_07