HRID579217

反应详情

EQUATION

反应方程式

HRID 579217 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 3 L volume four-necked flask, ethyl 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetate (9-a) (320.82 g) and tetrahydrofuran (600 ml) were added at room temperature and cooled. 10.7% by weight of aqueous sodium hydroxide solution (900 ml) was added dropwise at 10° C. over 2 hours. The resulting mixture was stirred at room temperature for 1 hour. After the organic solvent was removed under reduced pressure, tert-butyl methyl ether was added to the aqueous layer to wash. After the organic layer was removed, to the aqueous layer was added dropwise concentrated hydrochloric acid (180 ml), and extracted with tert-butyl methyl ether. The organic layer was concentrated under reduced pressure to give 166.55 g of 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetic acid (8-a).

WORKUP

后处理

  1. temperaturecooled
  2. customAfter the organic solvent was removed under reduced pressure, tert-butyl methyl ether
  3. additionwas added to the aqueous layer
  4. washto wash
  5. customAfter the organic layer was removed, to the aqueous layer
  6. additionwas added dropwise concentrated hydrochloric acid (180 ml)
  7. extractionextracted with tert-butyl methyl ether
  8. concentrationThe organic layer was concentrated under reduced pressure