反应详情

0.35 g of the crude 2-(3-fluoro-4-hydroxyphenyl)-5(4-n-hexylphenyl)pyrazine was dissolved in 3 ml of dimethyl sulfoxide and 3 ml of tetrahydrofuran. To the resulting solution, was added 0.12 g of potassium-tertbutoxide. The obtained mixture was stirred at room temperature for 30 minutes and then 0.22 g of n-nonyl bromide was added thereto. The mixture was stirred at room temperature for additional five hours. Then the reaction mixture was diluted with ethyl acetate, washed with dilute hydrochloric acid and with a 30% aqueous solution of sodium hydroxide and the repeatedly washed with water until the washing liquor showed a pH value of approximately 7. Then the ethyl acetate phase was dehydrated over sodium sulfate and the solvent was distilled off. Thus 0.48 g of a crude reaction product was obtained. The crude reaction product was purified by silica gel column chromatography and recrystallized from acetone. Thus 0.41 g of the title compound was obtained.

1. stirringThe mixture was stirred at room temperature for additional five hours
2. washwashed with dilute hydrochloric acid and with a 30% aqueous solution of sodium hydroxide
3. washthe repeatedly washed with water until the washing liquor
4. distillationthe solvent was distilled off
5. customThus 0.48 g of a crude reaction product
6. customwas obtained
7. customThe crude reaction product
8. customwas purified by silica gel column chromatography
9. customrecrystallized from acetone