HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Cesium carbonate → Alpha-[bis[(1,1-dimethylethoxy)carbonyl]amino]-2-oxo-4-(phenylmethoxy)1(2h)-pyridinepropanoic acid methyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | 4-Benzyloxy-2(1H)-pyridone | HCID 3607724 | — |
| Edukt | Methyl 2-(bis((tert-butoxy)carbonyl)amino)prop-2-enoate | HCID 10870342 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | Alpha-[bis[(1,1-dimethylethoxy)carbonyl]amino]-2-oxo-4-(phenylmethoxy)1(2h)-pyridinepropanoic acid methyl ester | HCID 58864469 | — |
Reaktionsbedingungen
| Temperatur | 80 °C |
|---|
Reaktionsschritte
To a solution of 2-(di-tert-butoxycarbonylamino)-acrylic acid methyl ester (900 mg, 3.0 mmol), and 4-benzyloxy-1H-pyridin-2-one (630 mg, 1.03 equiv) in acetonitrile (2.5 mL) was added cesium carbonate (100 mg, 0.10 equiv). The resulting suspension was heated to 80° C. via microwave for 2 h. The reaction was concentrated, dissolved in water, and extracted with methylene chloride (3×). The combined organic phases were washed with brine, dried over magnesium sulfate, and concentrated to give 1.47 g (97%) which was used without purification. Mass spec.: 503.56 (MH)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07220862B2 |
| Quelldatensatz | uspto-grants-2007_05 |
| ORD ID | ord-cf472808937e4b32a2c2e4fe5447d432 |
| Quellennotiz | uspto-grants-2007_05 |