反应详情

A mixture of 4-(4-carbomethoxyphenyl) butan-2-one (3.0 g) and 2-hydroxy-2-(3-trifluoromethylphenyl) ethanamine (3.0 g) in dry benzene (100 ml) was refluxed under Dean and Stark conditions for 2 hours. The solvent was replaced with methanol (100 ml) and sodium borohydride (2.0 g) was added portionwise with ice cooling. The mixture was stirred at ambient temperature for 2 hours, the solvent was evaporated and the residue was partitioned between water (100 ml) and chloroform (100 ml). The organic phase was dried (MgSO4) and evaporated to an oil, which was chromatographed on silica gel 60 in 3% methanol/chloroform. The title compound was obtained as a colourless oil.

1. temperaturewas refluxed under Dean and Stark conditions for 2 hours
2. additionwas added portionwise with ice cooling
3. customthe solvent was evaporated
4. customthe residue was partitioned between water (100 ml) and chloroform (100 ml)
5. dry with materialThe organic phase was dried (MgSO4)
6. customevaporated to an oil, which
7. customwas chromatographed on silica gel 60 in 3% methanol/chloroform