HRID1728855

反应详情

EQUATION

反应方程式

HRID 1728855 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound is prepared by the procedure of Example 27 using 2.55 g of product from Example 20, 0.999 g of product from Example 15, 0.319 g of washed 50% sodium hydride and 30 ml of tetrahydrofuran. The reaction is stirred at room temperature for hours, heated at reflux temperature for 24 hours; followed by stirring at room temperature for an additional 48 hours. The residue is purified by column chromatography (silica gel: 5% methyl alcohol/ethyl acetate) to give 0.862 g of the desired product. The spectral data indicates the presence of 2 rotomers.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux temperature for 24 hours
  3. stirringby stirring at room temperature for an additional 48 hours
  4. customThe residue is purified by column chromatography (silica gel: 5% methyl alcohol/ethyl acetate)