反应详情

In a nitrogen atmosphere, 1.51 g of sodium iodide is dissolved in 22 mL of acetonitrile. Then, 1.10 g of trimethylsilyl chloride is added thereto. The resulting solution is stirred at ambient temperature for 20 minutes. Then, 0.43 g of 6-fluoro-3-methoxy-2-pyrazinecarboxamide is added thereto. The resulting solution is stirred at the same temperature as above for 18 hours. Then, a mixture of 10 mL of water and 200 mL of chloroform is added to the reaction mixture, and separated into layers. The organic layer thus obtained is washed successively with 5% aqueous solution of sodium thiosulfate and saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate. The solvent is distilled off under reduced pressure. The residue thus obtained is purified by column chromatography (eluent: hexane:ethyl acetate=2:1) to obtain 0.06 g of 6-fluoro-3-hydroxy-2-pyrazinecarboxamide.

1. stirringThe resulting solution is stirred at the same temperature as above for 18 hours
2. additionis added to the reaction mixture
3. customseparated into layers
4. customThe organic layer thus obtained
5. washis washed successively with 5% aqueous solution of sodium thiosulfate and saturated aqueous solution of sodium chloride
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationThe solvent is distilled off under reduced pressure
8. customThe residue thus obtained
9. customis purified by column chromatography (eluent: hexane:ethyl acetate=2:1)