HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Acetate → 2,6-Dibromo-4-methylbenzaldehyde (2,4-difluorophenyl)hydrazone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Acetate | HCID 517045 | — |
| Edukt | 2,4-Difluorophenylhydrazine hydrochloride | HCID 2733301 | — |
| Edukt | 2,6-Dibromo-4-methylbenzaldehyde | HCID 12982748 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 2,6-Dibromo-4-methylbenzaldehyde (2,4-difluorophenyl)hydrazone | HCID 66648395 | 74,9% |
Reaktionsschritte
2,6-Dibromo-4-methylbenzaldehyde (89.5 g, 0.322 mol), (2,4-difluorophenyl)hydrazine hydrochloride (58.25 g, 0.322 mol) and sodium acetate (26.9 g, 0.328 mol) were heated in methanol (1.25 L) at reflux for 3.5 hours. The mixture was cooled and the precipitate was collected by filtration and partitioned between ethyl acetate (750 mL) and water (250 mL). The ethyl acetate layer was combined with a second ethyl acetate extract, washed successively with water and brine, dried over anhydrous sodium sulphate and evaporated under reduced pressure to afford the title compound as an off-white solid (97.5 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08093281B2 |
| Quelldatensatz | uspto-grants-2012_01 |
| ORD ID | ord-e509296f66724446bb0b4bcb87492c90 |
| Quellennotiz | uspto-grants-2012_01 |