HRID854958

反应详情

EQUATION

反应方程式

HRID 854958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
212.5 °C

PROCEDURE

实验过程

To a solution of 2-(3-methoxyphenyl)-2-methylpropanal (20.0 g, 112 mmoles) in 90 mL of N-methylpyrrolidinone was added thiophenol (11.5 mL, 112 mmoles) and anhydrous K2CO3 (1.55 g, 11.2 mmoles). The mixture was stirred at 210-215 ° C. for 3 h. After cooling, the mixture was partitioned between Et2O and 5% aqueous NaOH. The aqueous layer was acidified with dilute HCl and extracted with DCM. The combined organic extracts were dried over Na2SO4, filtered, and evaporated. Chromatography of the residue using 25% EtOAc—hexane as eluent gave the title compound, 10.3 g, as a pale yellow oil.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe mixture was partitioned between Et2O and 5% aqueous NaOH
  3. extractionextracted with DCM
  4. dry with materialThe combined organic extracts were dried over Na2SO4
  5. filtrationfiltered
  6. customevaporated