HRID328543

反应详情

EQUATION

反应方程式

HRID 328543 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

166 parts of triethyl phosphite are heated for 1 hour to 140° C in a nitrogen atmosphere with 2 parts of highly active Raney cobalt (Ra-Co-Lu). A mixture of 1 part of phenothiazine and 80 parts of allyl chloride is then added dropwise at 140° C. Once the reaction has started, the temperature may be lowered to 120° C. After 5.5 hours, 63 parts of ethyl chloride have distilled off and the mixture is deep blue in colour. Fractional distillation gives 135 parts of allyl phosphonic acid diethyl ester, corresponding to 76% of the theoretical yield.

WORKUP

后处理

  1. additionis then added dropwise at 140° C
  2. custommay be lowered to 120° C
  3. distillation63 parts of ethyl chloride have distilled off
  4. distillationFractional distillation