HRID1763974

反应详情

EQUATION

反应方程式

HRID 1763974 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.4 Parts of metallic sodium was dissolved in 50 parts of anhydrous methanol, and 5.5 parts of ethyl 3,3-dimethyl-4,6,6-trichloro-5-hexenoate prepared in the same manner as in Example 1 was added to the solution. The mixture was agitated for 2 hours under reflux of methanol. The liquid reaction mixture was naturally cooled, and 20 parts of water was added thereto and the mixture was agitated at 40° to 50° C. for 2 hours. Then, methanol was distilled under reduced pressure, and the residue was neutralized with hydrochloric acid and extracted with diethyl ether. The ether extract was dried and the ether was distilled to obtain 3.7 parts of the crystal of 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropane-carboxylic acid. The yield was 88 % based on ethyl 3,3-dimethyl-4,6,6-trichlorohexenoate.

WORKUP

后处理

  1. customprepared in the same manner as in Example 1
  2. additionwas added to the solution
  3. customThe liquid reaction mixture
  4. temperaturewas naturally cooled
  5. stirringthe mixture was agitated at 40° to 50° C. for 2 hours
  6. distillationThen, methanol was distilled under reduced pressure
  7. extractionextracted with diethyl ether
  8. extractionThe ether extract
  9. customwas dried
  10. distillationthe ether was distilled