HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → 4-Difluoro methoxy-8-nitro-1-formyl dibenzo[b,d]furan
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Sodium Acetate | HCID 517045 | — |
| Edukt | 4-Difluoromethoxy-3-(4-nitro-2-bromophenoxy)benzaldehyde | HCID 24758282 | — |
| Produkt | 4-Difluoro methoxy-8-nitro-1-formyl dibenzo[b,d]furan | HCID 21105710 | 73,3% |
Reaktionsschritte
To a mixture of 3-(2-bromo-4-nitrophenoxy)-4-(difluoromethoxy)benzaldehyde (11.5 g, 0.030 mol) and sodium acetate (3.7 g, 0.045 mol) in dimethylformamide (50 mL) palladium(II) acetate (0.68 g, 0.003 mol) was added in 4 different lots with 1 hour duration at 120-125° C. After the completion of the addition, it was refluxed for 16 hours. The reaction mixture was filtered through hyflo, washed with dimethylformamide (10 mL). The filtrate was poured into the cold water. The solid separated out was filtered. The solid was washed with hexane and dried. Yield—73.3%. HPLC (purity): 84.5%; Rf—0.5 (Ethyl acetate:Hexane (3:7)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08580795B2 |
| Quelldatensatz | uspto-grants-2013_11 |
| ORD ID | ord-e52a30bfcae64afbb41a65f52481ab92 |
| Quellennotiz | uspto-grants-2013_11 |