HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → HCID 21911050, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Benzoic acid, 2-fluoro-, ethyl ester | HCID 67953 | — |
| Edukt | Tert-butyl(4'-hydroxybiphenyl-3-ylmethyl)methylcarbamate | HCID 69643261 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylacetamide | HCID 31374 | — |
| Produkt | HCID 21911050 | HCID 21911050 | 104,9% |
Reaktionsschritte
2.15 g (12.8 mmol) of ethyl 2-fluorobenzoate and 1.9 g (14 mmol) of potassium carbonate are successively added to a solution of 4 g (12.8 mmol) of tert-butyl (4′-hydroxybiphenyl-3-ylmethyl)methylcarbamate in 45 ml of dimethylacetamide. The reaction medium is refluxed for 48 hours, cooled, diluted with water and extracted with ethyl acetate. The organic phase is dried over sodium sulfate, filtered and concentrated under vacuum. The residue obtained is purified by chromatography on a column of silica eluted with an 80/20 heptane/ethyl acetate mixture. 3.1 g of ethyl 2-{3′-[(tert-butoxycarbonylmethylamino)methyl]biphenyl-4-yloxy}benzoate are obtained in the form of a colorless oil, in a yield of 53%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07307078B2 |
| Quelldatensatz | uspto-grants-2007_12 |
| ORD ID | ord-cb2bf88750c64ea8856627e28cf92620 |
| Quellennotiz | uspto-grants-2007_12 |