反应详情

温度

60 °C

2-(8-Bromooctyl)-1,3-dioxolane (218 mg, 0.82 mmol) followed by di-isopropylethylamine (361 μL, 2.07 mmol) were added to a solution of piperidin-4-ylmethyl 2-cyclohexyl-2-hydroxy-2-phenylacetate hydrochloride (252 mg, 0.69 mmol) in acetonitrile (4 mL). The reaction mixture was heated at 60° C. for 17 hours. After this time, the reaction was cooled to RT and diluted with dichloromethane. The organic extracts were washed with water, filtered through a hydrophobic frit, and concentrated under reduced pressure. The crude material was purified by silica gel column chromatography eluting with 100% dichloromethane to 40:1 dichloromethane:methanol to afford the title compound that was used without further purification in the next step.

1. temperatureAfter this time, the reaction was cooled to RT
2. washThe organic extracts were washed with water
3. filtrationfiltered through a hydrophobic frit
4. concentrationconcentrated under reduced pressure
5. customThe crude material was purified by silica gel column chromatography
6. washeluting with 100% dichloromethane to 40:1 dichloromethane