反应详情

温度

70 °C

To a suspension of 1.1 g of 60% sodium hydride in 30 ml of dimethyl sulfoxide under stirring at 70° C. for 30 minutes was added 4.1 g of 4-(4-methylphenyl)butanol at room temperature and stirred for 30 minutes. To a mixture was added 40 ml of tetrahydrofuran and was cooled at 0° C. To the resulting mixture was added dropwise a solution of 3.9 g of 6-chloromethyl-2-formylpyridine in 40 ml of tetrahydrofuran. After completion of the addition, the mixture was stirred at the same temperature for 30 minutes and further was stirred at room temperature for 4 hours. After completion of the reaction, the reaction mixture was poured into water, extracted with ethyl acetate and washed with water. The organic layer was dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure to give a residue as an oily substance. The residue was purified by column chromatography on silica gel by passing chloroform and methanol(100:1 ) to give 1.3 g of 6-[4-(4-methylphenyl) butoxy]methyl-2-formylpyridine.

1. stirringstirred for 30 minutes
2. temperaturewas cooled at 0° C
3. additionAfter completion of the addition
4. stirringthe mixture was stirred at the same temperature for 30 minutes
5. stirringfurther was stirred at room temperature for 4 hours
6. customAfter completion of the reaction
7. extractionextracted with ethyl acetate
8. washwashed with water
9. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
10. distillationthe solvent was distilled off under reduced pressure
11. customto give a residue as an oily substance
12. customThe residue was purified by column chromatography on silica gel