HRID248015

反应详情

EQUATION

反应方程式

HRID 248015 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 5.0 g of product from Example 111, 0.683 g of washed 50% sodium hydride, 2.14 g of product from Example 12 and 100 ml of dry tetrahydrofuran. The reaction is stirred at room temperature for 1 hour, heated at reflux temperature for 18 hours and cooled to room temperature. The mixture is poured into water, extracted with chloroform and concentrated in vacuo. The residue is purified by column chromatography (silica gel: 15-30% ethyl acetate/hexane) to give 2.93 g of the desired product.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux temperature for 18 hours
  3. temperaturecooled to room temperature
  4. extractionextracted with chloroform
  5. concentrationconcentrated in vacuo
  6. customThe residue is purified by column chromatography (silica gel: 15-30% ethyl acetate/hexane)