反应详情

A solution of 150 mg (0.365 mmol) of methyl E-4-[3-(4-cyanobenzyl)-5-(2-hydroxyphenyl)pent-4-enyl]benzoate (enantiomer 1, Example 51A) in 3 ml of dry acetonitrile is mixed with 139 mg (0.47 mmol) of 1-(chloromethyl)-4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]benzene [prepared as described in EP 0 009 787-A2] and 100 mg (0.73 mmol) of anhydrous potassium carbonate and then heated under reflux for 12 h. The mixture is then filtered and the filtrate is evaporated to dryness. The residue is purified by chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 4:1). 210 mg (0.31 mmol, 86% of theory) of an oil are isolated.

1. temperatureheated
2. temperatureunder reflux for 12 h
3. filtrationThe mixture is then filtered
4. customthe filtrate is evaporated to dryness
5. customThe residue is purified by chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 4:1)
6. custom210 mg (0.31 mmol, 86% of theory) of an oil are isolated