HRID1003155

反应详情

EQUATION

反应方程式

HRID 1003155 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of ethyl 2-methoxyphenyiacetate (11.6 g), sodium tert-butoxide (12.7 g) and ethyl acetate (15.8 g) in diisopropylether was heated at 70° C. for 2.5 hours and stirred at room temperature overnight. Ethyl acetate and hydrochloric acid (2M) were added and the organic phase dried (magnesium sulphate) and evaporated. The residue was distilled in vacuo to give ethyl 2-(2-methoxyphenyl)acetoacetate as a liquid (8.5 g), NMR 1.15 and 1.13(t,3h), 1.8 and 2.2(s,3H), 3.75 and 3.85(s,3H), 4.1-4.3(2q,2H), 5.15(s,1H), 6.9-7.3(m,4H), 13.1(s,1H).

WORKUP

后处理

  1. dry with materialthe organic phase dried (magnesium sulphate)
  2. customevaporated
  3. distillationThe residue was distilled in vacuo