HRID65090

反应详情

EQUATION

反应方程式

HRID 65090 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3.96 g of 4-cyano-4-isopropyl-4-(3,4-dimethoxyphenyl)butyraldehyde and 2.00 g of 2-(4-methoxyphenoxy)ethylamine in 50 ml of ethanol was refluxed for 1 hour. To the solution was added 0.55 g of sodium borohydride under ice-cooling, and the solution was stirred for 30 minutes at room temperature. The solvent was removed and the residue was dissolved in 10% hydrochloric acid and washed with ether. The aqueous layer was made alkaline with potassium carbonate and extracted with ethyl acetate. The extract was washed with water, dried, and evaporated. The residue was chromatographed on silica gel using chloroform as an eluent to give 2.93 g of the desired compound as a pale yellow oil.

WORKUP

后处理

  1. temperaturecooling
  2. customThe solvent was removed
  3. dissolutionthe residue was dissolved in 10% hydrochloric acid
  4. washwashed with ether
  5. extractionextracted with ethyl acetate
  6. washThe extract was washed with water
  7. customdried
  8. customevaporated
  9. customThe residue was chromatographed on silica gel