反应详情

温度

115 °C

To a 2 ml N,N-dimethylformamide solution of 150 mg (0.36 mmol) of the compound obtained in Example 15, 8 mg (0.036 mmol) of palladium acetate, 22 mg (0.072 mmol) of tri-o-tolylphosphine, 0.15 ml (1.08 mmol) of triethylamine, and 97 μl (1.08 mmol) of methyl acrylate were added, and the mixture was stirred at 115° C. in a sealed tube for 15 hours. Then, the reaction mixture was cooled to room temperature, water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate, whereafter the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=2/1) to obtain 130 mg (85%) of the captioned compound.

1. temperatureThen, the reaction mixture was cooled to room temperature
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with water
4. dry with materiala saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate, whereafter the solvent
5. distillationwas distilled off under reduced pressure
6. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=2/1)