Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Diisopropyl Ether | HCID 7914 | — |
| Edukt | Phenylpropynoic acid methyl ester | HCID 138378 | — |
| Edukt | 1-(4-Fluorobenzoyl)pyrrolidine-2-carboxylic acid | HCID 12367684 | — |
| Lösungsmittel | Acetic Anhydride | HCID 7918 | — |
| Produkt | HCID 22335619 | HCID 22335619 | — |
Reaktionsschritte
Methyl phenylpropiolate (methyl dehydrocinnamate (0.96 g, 6 mmol)) is dissolved in acetic anhydride (14 ml) and brought to the boiling temperature of acetic anhydride in a hot oil bath (140° C.). The total amount of 1-(4-fluorobenzoyl)pyrrolidine-2-carboxylic acid (1.42 g, 6 mmol) is added, and the thoroughly mixed solution is refluxed (1 28° C.) for 20 h with stirring. After standing for 4 hours and cooling to RT, a pure crystalline solid deposits (TLC: Al2O3, diisopropyl ether, Rf 0.7). The crystals are filtered off with suction, washed with water (20 ml) and finally with isopropyl ether (10 ml). The dried crystals weigh 650 mg (32.5% of theory)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06936632B2 |
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| Quelldatensatz | uspto-grants-2005_08 |
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| ORD ID | ord-63c25cf1c97740d3a0ae2a9312f174b0 |
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| Quellennotiz | uspto-grants-2005_08 |
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