HRID345737

反应详情

EQUATION

反应方程式

HRID 345737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

16.3 g of anhydrous zinc chloride was dissolved in 10.3 g of S-(+)-2-methylbutanoic acid by heating to 110° C. 13.2 g of resorcinol was added to the mixture and then the temperature of the admixture was raised to 150° C. over a period of 30 minutes under stirring. The reaction mixture was then cooled to the room temperature, and a mixture composed of 25 ml of hydrochloric acid and 25 ml of water was added thereto. The reaction mixture was then subjected to extraction for three times, each by using 50 ml of ethyl ether. The extracts were joined together and rinsed with an aquesous solution of NaHCO3 for three times, and then rinsed with water for three times. Anhydrous Na2SO4 was added to the rinsed extract to dry the ethyl ether extract. Ethyl ether was removed to obtain a liquid reaction product which was refined through silica gel column chromatography while using chloroform as the eluent. As a result, 6.2 g of 3-hydroxy-4 -(1-oxo-2-methylbutyl)phenol was obtained.

WORKUP

后处理

  1. temperaturethe temperature of the admixture was raised to 150° C. over a period of 30 minutes
  2. temperatureThe reaction mixture was then cooled to the room temperature
  3. additionwas added
  4. extractionThe reaction mixture was then subjected to extraction for three times
  5. washrinsed with an aquesous solution of NaHCO3 for three times
  6. washrinsed with water for three times
  7. additionAnhydrous Na2SO4 was added to the rinsed
  8. extractionextract
  9. dry with materialto dry the ethyl ether
  10. extractionextract
  11. customEthyl ether was removed
  12. customto obtain
  13. customa liquid reaction product which