HRID485384

反应详情

EQUATION

反应方程式

HRID 485384 反应方程式

PROCEDURE

实验过程

A solution of 4-[3-[(dimethylamino)methyl]phenoxy]butanal (0.5 g) and 3-phenyl methyl-1H-1,2,4-triazole-5-amine (0.39 g) in dry toluene (60 ml) was heated under reflux during 3 h. The solvent was evaporated and replaced with methanol (50 ml). Sodium borohydride (0.4 g) was added and the mixture was stirred at 20° during 2 h. The methanol was evaporated and the residue partitioned between water and ethyl acetate. The organic extract was evaporated and the residue was purified by column chromatography to give the title compound, which crystallised from a mixture of ethyl acetate and cyclohexane as pale yellow crystals (0.09 g) m.p. 131°-3°; tlc system A,Rf 0.6.

WORKUP

后处理

  1. temperatureunder reflux during 3 h
  2. customThe solvent was evaporated
  3. additionSodium borohydride (0.4 g) was added
  4. customThe methanol was evaporated
  5. customthe residue partitioned between water and ethyl acetate
  6. extractionThe organic extract
  7. customwas evaporated
  8. customthe residue was purified by column chromatography