Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Malonic Acid | HCID 867 | — |
| Edukt | Piperidine | HCID 8082 | — |
| Edukt | 4-Ethoxybenzaldehyde | HCID 24834 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Produkt | 4-Ethoxycinnamic Acid | HCID 704218 | — |
Reaktionsschritte
A solution of 4-ethoxybenzaldehyde (1.00 mL, 7.20 mmol) and piperidine (0.11 mL, 1.08 mmol) in 40 mL of pyridine was heated to 120° C. A solution of malonic acid (1.50 g, 14.40 mmol) in 40 mL of pyridine was added dropwise over 30 min and the reaction solution was stirred at 120° C. for 4 h. After cooling down to 0° C., excess amount of concentrated HCl was added carefully to make ˜pH 1. A white crystalline precipitate formed, and the solid was collected by filtration, washed with 0.1 N HCl aqueous solution, and dried to afford compound 19 in 99.5% (1.40 g) of pure 19 as a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09115122B2 |
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| Quelldatensatz | uspto-grants-2015_08 |
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| ORD ID | ord-e34d4247259b419bbe12ceed44badcf1 |
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| Quellennotiz | uspto-grants-2015_08 |
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