HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → 2-(3,4-Dichlorophenoxy)-3-(dimethylamino)prop-2-enal
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Phosphorus oxychloride | HCID 24813 | — |
| Edukt | 1,2-Dichloro-4-(2,2-diethoxyethoxy)benzene | HCID 2782022 | — |
| Produkt | 2-(3,4-Dichlorophenoxy)-3-(dimethylamino)prop-2-enal | HCID 54555818 | — |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04558134 |
| Quelldatensatz | uspto-grants-1985_12 |
| ORD ID | ord-9a1fa99a01d84a3d9cf4b3a35aab1856 |
| Quellennotiz | uspto-grants-1985_12 |