反应详情

Dimethylformamide (29.2 g) was slowly added to 122.7 g of POCl3 in a reaction flask. After the addition was complete, the mixture was heated to 80° C. while 3,4-dichlorophenoxyacetaldehyde diethyl acetal (55.8 g) was added, and the resulting mixture was then heated for an additional two hours at about 80°-85° C. The reaction mixture was cooled to room temperature and poured into about 400 g of potassium carbonate in an ice-water mixture and then extracted with methylene chloride. The methylene chloride extract was then dried and concentrated to a dark oil which solidified upon dilution with ethyl acetate. 22.1 g of the desired, 2-(3,4-dichlorophenoxy)-3-dimethylamino-propenal was obtained and subsequently identified by NMR spectroscopy.

1. additionAfter the addition
2. additionwas added
3. temperaturethe resulting mixture was then heated for an additional two hours at about 80°-85° C
4. extractionextracted with methylene chloride
5. extractionThe methylene chloride extract
6. customwas then dried
7. concentrationconcentrated to a dark oil which