HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 2-(4-Chloro-3-sulfamoylbenzoyl)-benzo[b]furan
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Salicylaldehyde | HCID 6998 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Bromo-4'-chloro-3'-sulfamoylacetophenone | HCID 12952390 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 2-(4-Chloro-3-sulfamoylbenzoyl)-benzo[b]furan | HCID 21316593 | — |
Reaktionsschritte
4 g 2-Bromo-4'-chloro-3'-sulfamoylacetophenone and 1.63 g salicylaldehyde are maintained for 2 hours with agitation and with exclusion of moisture at a temperature of 80° C. in 50 ml anhydrous dimethyl formamide, in the presence of 2.9 g potassium carbonate ground under anhydrous conditions. After cooling, the batch is poured into a mixture of icewater and excess hydrochloric acid, extracted with ethyl acetate and dried over sodium sulfate. After having distilled off the solvent, crystallization is carried out from di-isopropyl ether and isopropanol. M.p. 152°-156° C. Recrystallization from glacial acetic acid after clarification with active charcoal gives colorless crystals having a melting point of 167°-170° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04156732 |
| Quelldatensatz | uspto-grants-1979_05 |
| ORD ID | ord-be87ce7bc2cb4532b71c9d0edfccb620 |
| Quellennotiz | uspto-grants-1979_05 |