HRID1383355

反应详情

EQUATION

反应方程式

HRID 1383355 的结构方程式

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A solution of 3-methoxy-5-methylphenylacetonitrile (9 g; 0.06 mol; from step (ii) above) and KOH (17 g; 0.3 mol) in 150 mL of water:i-PrOH (2:1) was heated while stirring in an autoclave at 120° C. overnight and then at room temperature for 2 days. The reaction mixture was concentrated and extracted with ether. The aqueous phase was acidified and extracted twice with ether. The combined organic layers were washed with water, dried (Na2SO4), and evaporated to a residue which was dissolved in EtOH, treated with activated carbon, filtered, and evaporated to yield the sub-title compound (8.1 g; 80%) as yellow crystals.

WORKUP

后处理

  1. waitat room temperature for 2 days
  2. concentrationThe reaction mixture was concentrated
  3. extractionextracted with ether
  4. extractionextracted twice with ether
  5. washThe combined organic layers were washed with water
  6. dry with materialdried (Na2SO4)
  7. customevaporated to a residue which
  8. dissolutionwas dissolved in EtOH
  9. additiontreated with activated carbon
  10. filtrationfiltered
  11. customevaporated