反应详情

To the above crude 2-fluoro-5-(4-fluorophenyl)-5-methylhex-1-en-3-ol (1.73 g, 7.65 mmol) stirred under nitrogen gas and cooled on ice, was added diethyl zinc (1.1 M in toluene, 8.0 mL). After 5 minutes, 1.0 mL of diiodomethane was added dropwise over 20 minutes and the mixture was stirred and allowed to come to room temperature and then stirred at room temperature for 4 days. 0.5 mL of water was then added to the reaction mixture, followed by ethyl acetate. The resulting mixture was then filtered through diatomaceous earth and the solvent was removed in vacuo and the residue was fractionated over silica gel (hexanes-dichloromethane (1:1) to dichloromethane gradient) to give 1-(1-fluorocyclopropyl)-3-(4-fluorophenyl)-3-methylbutan-1-ol as an oil.

1. temperaturecooled on ice
2. customto come to room temperature
3. stirringstirred at room temperature for 4 days
4. filtrationThe resulting mixture was then filtered through diatomaceous earth
5. customthe solvent was removed in vacuo