HRID596988

反应详情

EQUATION

反应方程式

HRID 596988 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The ethyl 2-((3,5-di-tert-butyl-4-hydroxyphenyl)thio)hexanoate product (75 grams; 0.195 mole) obtained in Example 2 was dispersed in 300 ml. of 95% ethanol and 500 ml. of 5N potassium hydroxide added thereto. The resulting reaction mixture was heated on a steam bath at the boiling point under gentle reflux for about 90 minutes with occasional stirring. Following the heating period, the reaction mixture was poured into 2000 ml. of 5% HCl with vigorous stirring. The white precipitate formed upon acidification was obtained by filtration and washed with water. Recrystallization (twice) of the precipitate from a methylene chloride-hexane mixture gave the desired 2-((3,5-di-tert-butyl-4-hydroxyphenyl)thio)hexanoic acid compound having a melting point of 140°-142° C.

WORKUP

后处理

  1. additionwas dispersed in 300 ml
  2. customThe resulting reaction mixture
  3. temperaturewas heated on a steam bath at the boiling point
  4. temperatureunder gentle reflux for about 90 minutes with occasional stirring
  5. additionthe reaction mixture was poured into 2000 ml
  6. customThe white precipitate formed upon acidification
  7. customwas obtained by filtration
  8. washwashed with water
  9. customRecrystallization (twice) of the precipitate from a methylene chloride-hexane mixture