反应详情

温度

85 °C

100 mg (0.25 mmol) of the compound from Example 99A, 53 mg (0.49 mmol) of o-cresol and 91 mg (0.74 mmol) of 4-N,N-dimethylaminopyridine were dissolved in 5 ml of acetonitrile, and 39 mg (0.62 mmol) of copper powder and 49 mg (0.62 mmol) of copper(II) oxide were added. The mixture was stirred at 85° C. for 16 h. For work-up, the mixture was cooled to RT and filtered through silica gel, and the residue was rinsed with a little ethyl acetate. The filtrate was concentrated under reduced pressure and the crude product was then purified chromatographically [Method 19]. This gave 25 mg (23% of theory) of the target compound.

1. temperatureFor work-up, the mixture was cooled to RT
2. filtrationfiltered through silica gel
3. washthe residue was rinsed with a little ethyl acetate
4. concentrationThe filtrate was concentrated under reduced pressure
5. customthe crude product was then purified chromatographically [Method 19]