反应详情

温度

85 °C

2400 g (39 mol) of ethylene glycol, 430 g (3.62 mol) of trimethyl orthoformate, 550 g (3.9 mol) of pentane-2,3,4-trione 3-(O-methyloxime) and 9 g of p-toluene sulfonic acid (46 mmol) were heated with stirring to 85° C. over a period of 15 min. After 30 min at 85° C., the mixture was cooled to room temperature. During the reaction, volatile components were distilled off via a column head. For work-up, the mixture was washed with saturated sodium bicarbonate solution and extracted with methyl tert-butyl ether, and the combined organic phases were washed twice with water and finally dried over magnesium sulfate. Distillative removal of the solvent gave 580 g of a red-brown oil (phys. data see Tab. 1).

1. waitAfter 30 min at 85° C.
2. temperaturethe mixture was cooled to room temperature
3. customDuring the reaction, volatile components
4. distillationwere distilled off via a column head
5. washFor work-up, the mixture was washed with saturated sodium bicarbonate solution
6. extractionextracted with methyl tert-butyl ether
7. washthe combined organic phases were washed twice with water
8. dry with materialfinally dried over magnesium sulfate
9. customDistillative removal of the solvent