HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triphenylphosphine → N-[3-(3-methyl-but-3-enyloxy)-phenyl]-acetamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Edukt | 3-Hydroxyacetanilide | HCID 12124 | — |
| Edukt | 3-Methyl-3-buten-1-ol | HCID 12988 | — |
| Edukt | Diethyl azodicarboxylate | HCID 5462977 | — |
| Edukt | Acetic acid 3-formylamino-phenyl ester | HCID 57470213 | — |
| Lösungsmittel | Benzene | HCID 241 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | N-[3-(3-methyl-but-3-enyloxy)-phenyl]-acetamide | HCID 57567384 | 52% |
Reaktionsschritte
A suspension of the mixture of N-(3-hydroxy-phenyl)-acetamide and acetic acid 3-formylamino-phenyl ester (18.12 g, 0.12 mol), 3-methyl-but-3-en-1-ol (8.6 g, 0.1 mol), DEAD (87 g, 0.2 mol) and Ph3P (31.44 g, 0.12 mol) in benzene (250 mL) was heated at reflux overnight and then cooled to room temperature. The reaction mixture was poured into water and the organic layer was separated. The aqueous phase was extracted with EtOAc (300×3 mL). The combined organic layers were washed with brine, dried over anhydrous Na2SO4 and concentrated. The residue was purified by column chromatography to give N-[3-(3-methyl-but-3-enyloxy)-phenyl]-acetamide (11 g, 52%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08829204B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-e10579a39eec48f0b3a2326d7aaaf826 |
| Quellennotiz | uspto-grants-2014_09 |