反应详情

A solution of 1-(4-Bromo-phenyl)-3-chloro-propan-1-ol* (1.5 g, 6.01 mmol) and imidazole (1.23 g, 18.03 mmol) in dimethylformamide (18 ml) was heated at 100° C. for 18 hrs then partitioned between water and ethyl acetate. The organic extracts were combined, dried (MgSO4), filtered, concentrated and purified by column chromatography (SiO2), eluting with methanol:dichloromethane (2:98) to methanol:dichloromethane (6:94) to afford the title compound (0.75 g, 44% yield). LC/MS: (PS-B3) Rt 2.48 [M+H]+ 281.14, 283.11. *This starting material can be made by the method described in Example 43A.

1. customthen partitioned between water and ethyl acetate
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated
5. custompurified by column chromatography (SiO2)
6. washeluting with methanol:dichloromethane (2:98) to methanol:dichloromethane (6:94)