反应详情

温度

112.5 °C

In 86 mL of dimethyl sulfoxide was dissolved 4.3 g of N-(5-bromo-3-cyano-2-pyrazinyl)benzamide. After adding 8.3 g of potassium fluoride, the mixture thus obtained was stirred at 110-115° C. for one hour. The reaction mixture was returned to room temperature, a mixture of 100 mL of ethyl acetate and 200 mL of water was added, and the organic layer was separated. The organic layer thus obtained was washed successively with water and saturated aqueous solution of sodium chloride, treated with active charcoal and dried on anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [eluent: toluene:ethyl acetate=5:1] to obtain 0.47 g of N-(3-cyano-5-fluoro-2-pyrazinyl)benzamide as a white-colored solid product.

1. customthe mixture thus obtained
2. customwas returned to room temperature
3. additionwas added
4. customthe organic layer was separated
5. customThe organic layer thus obtained
6. washwas washed successively with water and saturated aqueous solution of sodium chloride
7. additiontreated with active charcoal
8. dry with materialdried on anhydrous magnesium sulfate
9. customthe solvent was removed under reduced pressure
10. customThe residue thus obtained
11. customwas purified by silica gel column chromatography [eluent: toluene:ethyl acetate=5:1]