反应详情

The reaction mixture of 128 mg (0.255 mmol) of 3-{1-[bis(4-chlorophenyl)methyl]azetidin-3-yl}-3-(3,5-difluorophenyl)-3-hydroxy-2,2-dimethylpropanenitrile and 3 mL of phosphorus oxychloride in 5 mL of pyridine was heated at reflux for 48 h. The solution was concentrated, poured into 30 mL of ether, and washed with 5 mL of aq NaHCO3. The organic layer was dried over Na2SO4 and concentrated. The residue was purified by silica gel chromatography with hexanes/ethyl acetate=4:1 to afford the title compound. 1NMR(CDCl3) δ 1.47 (s, 6H), 3.48 (s, 2H), 4.18 (s, 2H), 4.47 (s, 1H), 6.66-6.77 (m, 2H), 7.25-6-7.35 (m, 8H); Mass Spectrum: m/e=483 (M+1 35Cl, 35Cl) and 485 (M+1 35Cl, 37Cl).

1. temperaturewas heated
2. temperatureat reflux for 48 h
3. concentrationThe solution was concentrated
4. additionpoured into 30 mL of ether
5. washwashed with 5 mL of aq NaHCO3
6. dry with materialThe organic layer was dried over Na2SO4
7. concentrationconcentrated
8. customThe residue was purified by silica gel chromatography with hexanes/ethyl acetate=4:1