反应详情

A suspension of 5-bromo-2-(4-{[tert-butyl(dimethyl)silyl]oxy}cyclohex-1-en-1-yl)-3-methylpyridine (5.59 g) of Reference Example 110(1), benzophenonimine (2.77 g), palladium acetate (41 mg), (±)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (114 mg) and sodium tert-butoxide (2.1 g) in toluene (30 ml) was stirred under reflux for two hours. After completion of the reaction, the reaction solution was left stand, concentrated hydrochloric acid (20 ml) and water (60 ml) were added and stirred at room temperature for two hours. Then, diethyl ether was added and extracted with 1N hydrochloric acid aqueous solution. The resulting aqueous layer was cooled with ice, adjusted to pH>10 by the addition of 4N aqueous solution of sodium hydroxide and extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate and concentrated to give the titled compound (2.52 g) as a yellow solid.

1. temperatureunder reflux for two hours
2. customAfter completion of the reaction
3. additionwere added
4. stirringstirred at room temperature for two hours
5. extractionextracted with 1N hydrochloric acid aqueous solution
6. temperatureThe resulting aqueous layer was cooled with ice
7. additionadjusted to pH>10 by the addition of 4N aqueous solution of sodium hydroxide
8. extractionextracted with chloroform
9. dry with materialThe organic layer was dried over anhydrous sodium sulfate
10. concentrationconcentrated