反应详情

温度

0 °C

To a suspension of sodium hydride (60% in oil, 1.90 g, 47.5 mmol) in dry DMF (60 ml) was added dropwise a solution of the compound (3) (5.98 g, 36.2 mmol) obtained above in DMF (40 ml) under nitrogen atmosphere under ice-cooling. The mixture was stirred at 0° C. for 30 minutes, and thereto was added dropwise chloromethyl methyl ether (3.6 ml, 47.4 mmol). The reaction mixture was stirred at 0° C.-room temperature for 2 hours. The reaction mixture was poured into water, extracted with ethyl acetate, washed with saturated brine, dried over anhydrous magnesium sulfate and evaporated. The concentrate was purified by column chromatography on silica gel to give the title aldehyde compound (Compound A) as yellow liquid. Yield 7.17 g (95%).

1. temperaturecooling
2. stirringThe reaction mixture was stirred at 0° C.-room temperature for 2 hours
3. extractionextracted with ethyl acetate
4. washwashed with saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customevaporated
7. customThe concentrate was purified by column chromatography on silica gel