HRID1760169

反应详情

EQUATION

反应方程式

HRID 1760169 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.9 g of sodium hydride were initially introduced into 150 ml of cyclohexane, and a solution of 15 g of 1-(3,4-dimethoxyphenyl)ethanone in 16.3 ml of ethyl acetate was added. The reaction solution was boiled at 80° C. for 1 h, after which acetic acid was added and the whole was extracted with MTB-ether. The MTB-ether phase was dried over magnesium sulfate and subjected to rotary evaporation. The residue was chromatographed through silica gel (ethyl acetate/heptane 1/6). The following was obtained: 41 C12H14O4 (222.24); MS (ESI) 223 (M+H)

WORKUP

后处理

  1. customfor 1 h
  2. extractionthe whole was extracted with MTB-ether
  3. dry with materialThe MTB-ether phase was dried over magnesium sulfate
  4. customsubjected to rotary evaporation
  5. customThe residue was chromatographed through silica gel (ethyl acetate/heptane 1/6)
  6. customThe following was obtained