Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Ethyl phenylacetate | HCID 7590 | — |
| Edukt | Ethyl formate | HCID 8025 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | HCID 178509258 | HCID 178509258 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | HCID 178515326 | HCID 178515326 | — |
Reaktionsschritte
To tetrahydrofuran suspension of 480 mg of 60% sodium hydride, 2 ml of ethyl formate and 1.64 g of ethyl phenylacetate were added in nitrogen atmosphere, and stirred for 19 hours at room temperature. Adding 1.0 g of 3-amino-4-(4-phenylthiophenyl)pyrazole, the mixture was stirred for 4 hours under reflux. After allowing to cool, water and 10% hydrochloric acid was added. The solution obtained was extracted with ethyl acetate. After washing with water, the organic layer was dried over anhydrous sodium sulfate, and the solvent is distilled off. The residue was dissolved in 5 ml of acetic acid, and the mixture was heated and stirred for 2 to 20 hours at 120° C. After allowing to cool, ethyl acetate was added, and the precipitate was filtered. The filtrate was washed with ethyl acetate and ether and dried, and the title compound was obtained (270 mg, 18%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US05420128 |
|---|
| Quelldatensatz | uspto-grants-1995_05 |
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| ORD ID | ord-1eeb9566299843d08dca2af3b8d922f8 |
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| Quellennotiz | uspto-grants-1995_05 |
|---|