HRID1646173

反应详情

EQUATION

反应方程式

HRID 1646173 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of the diethyl[[2(bromomethyl)phenyl]methyl]phosphonate (Example A) (0.9 g, 2.8 mmol) in methanol (25 ml) and triethylamine (5 ml) is treated with glycine methyl ester hydrochloride (0.71 g, 5.6 mmol) and heated at reflux in an oil bath for 19 hours. The solvent is removed in vacuo and the residue dissolved in water and extracted with chloroform. The chloroform layer is dried over magnesium sulfate, filtered, and evaporated. The oily residue is purified via silica gel chromatography (2-4% methanol in chloroform as eluant).

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux in an oil bath for 19 hours
  3. customThe solvent is removed in vacuo
  4. dissolutionthe residue dissolved in water
  5. extractionextracted with chloroform
  6. dry with materialThe chloroform layer is dried over magnesium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. customThe oily residue is purified via silica gel chromatography (2-4% methanol in chloroform as eluant)