反应详情

0.80 g (2.42 mM) of 2-decyl-5-(3-fluoro-4-hydroxyphenyl)pyrimidine was dissolved in 10 ml of pyridine. Under stirring on an ice water bath, 0.62 ml (4.00 mM) of heptanoyl chloride was added dropwise to the above solution, followed by stirring for 15 minutes on the ice water bath and further stirring for 20 minutes at 45°-56° C. on a water bath. After the reaction, the reaction mixture was poured into 150 ml of ice water to precipitate a crystal. The crystal was recovered by filtration and washed with water. The washed crystal was dissolved in toluene and washed with water, followed by drying with anhydrous sodium sulfate and distilling-off of the solvent under reduced pressure. The residue was purified by silica gel column chromatography (eluent: toluene) and recrystallized two times from a mixture solvent of acetone-methanol to obtain 0.66 g of 2-decyl-5-(3-fluoro-4-heptanoyloxyphenyl)pyrimidine (Yield: 61.6%). ##STR26##

1. stirringfurther stirring for 20 minutes at 45°-56° C. on a water bath
2. customAfter the reaction
3. customto precipitate a crystal
4. filtrationThe crystal was recovered by filtration
5. washwashed with water
6. dissolutionThe washed crystal was dissolved in toluene
7. washwashed with water
8. dry with materialby drying with anhydrous sodium sulfate and distilling-off of the solvent under reduced pressure
9. customThe residue was purified by silica gel column chromatography (eluent: toluene)
10. customrecrystallized two times from a mixture solvent of acetone-methanol