反应详情

43.6 g (246 mmol) of 4,6-dichloropyrimidine-5-carboaldehyde was dissolved in 200 ml of methanol, and 120 g (622 mmol) of 28% sodium methoxide was added under cooling with ice and then reacted for 2 hours at room temperature. After completion of the reaction, the solvent was distilled off, and an aqueous citric acid solution was added, followed by extraction with ethyl acetate. The organic layer was washed with an aqueous sodium hydrogencarbonate solution, an aqueous citric acid solution, water and an aqueous sodium chloride solution in this order, dried and concentrated, and the obtained crude crystals were washed with isopropyl ether to obtain 8.3 g (yield: 20%) of 4,6-dimethoxypyrimidine-5-carboaldehyde.

1. temperatureunder cooling with ice
2. customreacted for 2 hours at room temperature
3. customAfter completion of the reaction
4. distillationthe solvent was distilled off
5. additionan aqueous citric acid solution was added
6. extractionfollowed by extraction with ethyl acetate
7. washThe organic layer was washed with an aqueous sodium hydrogencarbonate solution
8. dry with materialan aqueous citric acid solution, water and an aqueous sodium chloride solution in this order, dried
9. concentrationconcentrated
10. customthe obtained crude crystals
11. washwere washed with isopropyl ether