反应详情

BINAP (293 mg, 0.47 mmol) and Pd(OAc)2 (317 mg, 1.4 mmol) was added to a mixture of 2,8-diazaspiro[4.5]decane-8-carboxylic acid tert-butyl ester (5.66 g, 23.6 mmol), 4-bromopyridine HCl (4.58 g; 23.6 mmol) and sodium tert-butylate (6.8 g, 70.8 mmol) in toluene and the reaction mixture was degassed under argon for 20 minutes and heated under reflux for 4 h. The mixture was then diluted with ethyl acetate, stirred for 15 minutes and filtered over Celite. The organic phase was washed with water and sat. NaCl solution, dried over sodium sulfate and concentrated under reduced pressure. The crude product was purified by column chromatography. Yield: 53%

1. customthe reaction mixture was degassed under argon for 20 minutes
2. temperatureheated
3. temperatureunder reflux for 4 h
4. additionThe mixture was then diluted with ethyl acetate
5. filtrationfiltered over Celite
6. washThe organic phase was washed with water and sat. NaCl solution
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated under reduced pressure
9. customThe crude product was purified by column chromatography