HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → HCID 23024748, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 4-Benzyloxybenzyl chloride | HCID 70042 | — |
| Edukt | HCID 178469912 | HCID 178469912 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 23024748 | HCID 23024748 | 80,2% |
Reaktionsschritte
Sodium hydride (60%, oily, 1.85 g) was added to a mixture of 4-benzyloxybenzyl chloride (10.8 g), ethyl 3-phenyl-1H-pyrazole-4-carboxylate (10.0 g) and N,N-dimethylformamide (50 ml) at 0° C., and the mixture was stirred for 1.5 hours. The reaction mixture was poured into water, which was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium chloride solution, dried (MgSO4), then concentrated. The colorless crystals obtained were collected by filtration to yield ethyl 1-(4-benzyloxybenzyl)-3-phenyl-1H-pyrazole-4-carboxylate (15.3 g, yield: 80%). This was crystallized from ethyl acetate-diisopropyl ether. Melting point: 102–103° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07179823B1 |
| Quelldatensatz | uspto-grants-2007_02 |
| ORD ID | ord-0a2b5a2dcd9a493399ef20655b944712 |
| Quellennotiz | uspto-grants-2007_02 |