反应详情

A mixture of 263 mg (0.86 mmol) of 3-[bromo(4-chlorophenyl)methyl]benzonitrile, 213 mg (0.574 mmol) of 3-[1-(3,5-difluorophenyl)-2,2-dimethylpropyl]azetidine and 300 uL (1.72 mmol) of N,N-diisopropylethylamine in 6 mL of acetonitrile was heated to reflux for 3 h. Then the solution was concentrated and the residue was dissolved in 5 mL of hexane/ether. 1.5 mL of 1N HCl in ether was added to above solution to make salt. It was filtered and washed with hexane/ether. The residue was neutralized with base and was purified by silica gel chromatography with hexanes/ethyl acetate to afford one racemic diastereomer of the title compound; Mass Spectrum: m/e=465 (M+1 35Cl) and 467 (M+1 37Cl).

1. temperaturewas heated
2. temperatureto reflux for 3 h
3. concentrationThen the solution was concentrated
4. dissolutionthe residue was dissolved in 5 mL of hexane/ether
5. addition1.5 mL of 1N HCl in ether was added to above solution
6. filtrationIt was filtered
7. washwashed with hexane/ether
8. customwas purified by silica gel chromatography with hexanes/ethyl acetate