HRID582806

反应详情

EQUATION

反应方程式

HRID 582806 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl chloracetate (100 g, 99% pure, 0.81 mol) in ethanol is treated with ethanolic sodium ethoxide (282.9 g, 20.6% solution, 0.86 mole NaOC2H5) over a 1 hr period at 20° C.-30° C., heated at 40° C.-45° C. for 0.5 hr, cooled to room temperature, treated with diatomaceous earth, stirred for 0.25 hr and filtered. The filtercake is washed with ethanol. The combined filtrates are distilled to obtain the title product as a colorless liquid 75.78 g, 98.8% pure (71% yield), bp 87° C.-88° C./59 mmHg, identified by 13CNMR, 1HNMR and mass spectral analyses.

WORKUP

后处理

  1. temperatureheated at 40° C.-45° C. for 0.5 hr
  2. additiontreated with diatomaceous earth
  3. filtrationfiltered
  4. washThe filtercake is washed with ethanol
  5. distillationThe combined filtrates are distilled