反应详情

温度

10 °C

Under an argon atmosphere, to a mixture of 2-(4,4-dimethylcyclohexyl)ethanol (25.3 g) and DCM (200 mL) were added DMSO (50 mL) and TEA (100 mL), and a sulfur trioxide-pyridine complex (77.7 g) was added in small divided portions while maintaining the inner temperature to 10° C. or lower under ice-cooling. After stirring at room temperature for 2 hours, to the reaction mixture was added ice water, followed by concentration under reduced pressure and then extraction with chloroform. The organic layer was washed sequentially with 1 M hydrochloric acid and brine. To the organic layer was added MgSO4, followed by stirring. Then, the mixture was filtered and concentrated under reduced pressure to obtain (4,4-dimethylcyclohexyl)acetaldehyde (27.3 g).

1. additiona sulfur trioxide-pyridine complex (77.7 g) was added
2. temperaturelower under ice-cooling
3. concentrationfollowed by concentration under reduced pressure
4. extractionextraction with chloroform
5. washThe organic layer was washed sequentially with 1 M hydrochloric acid and brine
6. additionTo the organic layer was added MgSO4
7. stirringby stirring
8. filtrationThen, the mixture was filtered
9. concentrationconcentrated under reduced pressure