反应详情

A mixture of 1-(4-acetylphenyl) propan-2-one (10.9 g) and 2-hydroxy-2-phenylethanamine (8.5 g) in benzene (200 ml) was refluxed for 4 hours under Dean and Stark conditions. The solvent was replaced with ethanol (200 ml), platinum oxide (200 mg) was added and the mixture was hydrogenated at ambient temperature and pressure for 6 hours. The solution was filtered and the filtrate was evaporated and chromatographed on silica gel 60 (400 g) eluting with 1% methanol/chloroform. The first fraction (9.0 g) was crystallised from ether to give the title compound as a 9:91 mixture of diasteroisomers m.p. 120°-135°.

1. temperaturewas refluxed for 4 hours under Dean and Stark conditions
2. additionwas added
3. customwas hydrogenated at ambient temperature
4. filtrationThe solution was filtered
5. customthe filtrate was evaporated
6. customchromatographed on silica gel 60 (400 g)
7. washeluting with 1% methanol/chloroform
8. customThe first fraction (9.0 g) was crystallised from ether