HRID2309558

反应详情

EQUATION

反应方程式

HRID 2309558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 10.9 g. of ethyl-7-(1'-methoxycarbonyl-5'-oxocyclopentyl)-heptanoate in 100 ml. of distilled water containing 6 g. of conc. sulfuric acid was refluxed under nitrogen. Progress of the reaction was followed by gas chromatography/mass spectroscopy analysis of a sample at intervals. After 48 hours the reaction was virtually complete and the mixture was cooled and extracted with one volume of ethyl ether. The aqueous layer was separated and extracted and extracted again with one volume of ether and the combined ethereal extracts were dried over magnesium sulfate and evaporated to a colorless oil which was sufficiently pure for the next step in the process. Yield was 6.6 g., about 99%.

WORKUP

后处理

  1. additionA suspension of 10.9 g
  2. temperaturethe mixture was cooled
  3. extractionextracted with one volume of ethyl ether
  4. customThe aqueous layer was separated
  5. extractionextracted
  6. extractionextracted again with one volume of ether
  7. dry with materialthe combined ethereal extracts were dried over magnesium sulfate
  8. customevaporated to a colorless oil which