Реакция #1177

ord-33cc46ae4b86423a92b024e4bd6cb9eb

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reaction mixture is heated
  2. 2
    Температураto reflux for 7 hours
  3. 3
    workup.WAITleft

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05723483uspto-grants-1998_03