反应详情

To a stirred solution of 2,4-dichloro-6-hydroxybenzaldehyde (1.85 g; 9.7 mmol) in 20 mL DMF at ambient temperature was added solid potassium carbonate (1.47 g; 10.6 mmol), and the resulting yellow mixture was stirred at ambient temperature. After 30 minutes, iodomethane (5.5 g; 38.7 mmol) was added, and the resulting mixture was stirred in an oil bath set to 50° C. After 10 minutes, the reaction was determined to be complete by thin layer chromatography (90/10 hexane/EtOAc). After a total of 30 minutes the mixture was cooled to ambient temperature and diluted with 200 mL water. After stirring for a few minutes, the precipitate that formed was collected by filtration, washed with water, and dried under vacuum to give 1.93 g of 2,4-dichloro-6-methoxybenzaldehyde as an off-white powder.

1. stirringthe resulting mixture was stirred in an oil bath
2. customset to 50° C
3. waitAfter 10 minutes
4. temperatureAfter a total of 30 minutes the mixture was cooled to ambient temperature
5. stirringAfter stirring for a few minutes
6. customthe precipitate that formed
7. filtrationwas collected by filtration
8. washwashed with water
9. customdried under vacuum