反应详情

温度

100 °C

A mixture of 4-(4-bromo-phenyl)-1-methanesulfonyl-1,2,3,6-tetrahydro-pyridine (23.50 g, 74.32 mmol), potassium hydroxide (14.72 g, 222.95 mmol), 2-di-tert-butylphosphino-2′,4′,6′-tri-i-propyl-1,1′-biphenyl (2.52 g, 5.95 mmol) and tris(dibenzylideneacetone)dipalladium (0) (1.36 g, 1.49 mmol) is purged with nitrogen, and then deoxygenated 1,4-dioxane (150 mL) and deoxygenated water (150 mL) are added. The mixture is stirred at 100° C. for 1 h. The mixture is cooled to 23° C. and 1 M aq hydrochloric acid is added until pH 2-3. The aqueous layer is extracted with ethyl acetate. The organic layers are combined, dried over anhydrous sodium sulfate, filtered, and the solvent is removed to obtain a red solid. Diethyl ether is added and the solid is filtered to obtain 16 g of the title compound as an off-white solid. MS (m/z) 254 (M+1).

1. customis purged with nitrogen
2. customdeoxygenated 1,4-dioxane (150 mL) and deoxygenated water (150 mL)
3. additionare added
4. temperatureThe mixture is cooled to 23° C.
5. addition1 M aq hydrochloric acid is added until pH 2-3
6. extractionThe aqueous layer is extracted with ethyl acetate
7. dry with materialdried over anhydrous sodium sulfate
8. filtrationfiltered
9. customthe solvent is removed
10. customto obtain a red solid
11. filtrationthe solid is filtered