HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 1478174Erstellt: 26. Oktober 2026
Dithiaoctanediol → (Z)-N-(2-Cyclohexyl-1,5-dimethyl-3-oxo-2,3-dihydro-1H-pyrazol-4-yl)-5-(3,3-dimethylbut-1-en-1-yl)-4-methylisoxazole-3-carboxamide
https://huagongshe.com/reaction/1478174
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Dithiaoctanediol | HCID 78904 | — |
| Edukt | N-(2-Cyclohexyl-1,5-dimethyl-3-oxo-2,3-dihydro-1H-pyrazol-4-yl)-5-(3,3-dimethylbut-1-yn-1-yl)-4-methylisoxazole-3-carboxamide | HCID 118511150 | — |
| Katalysator | Palladium | HCID 23938 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | (Z)-N-(2-Cyclohexyl-1,5-dimethyl-3-oxo-2,3-dihydro-1H-pyrazol-4-yl)-5-(3,3-dimethylbut-1-en-1-yl)-4-methylisoxazole-3-carboxamide | HCID 118511121 | — |
Reaktionsschritte
N-(2-Cyclohexyl-1,5-dimethyl-3-oxo-2,3-dihydro-1H-pyrazol-4-yl)-5-(3,3-dimethylbut-1-yn-1-yl)-4-methylisoxazole-3-carboxamide (Example 7, Step 3)) (30 mg, 0.075 mmol) in EtOAc (3 mL) was treated with 2,2′-(ethane-1,2-diylbis(sulfanediyl))diethanol (13.72 mg, 0.075 mmol) and Pd-5% Barium sulphate (16.02 mg, 7.53 μmol). The mixture was degassed, thoroughly refilling with nitrogen and the mixture was stirred under an atmosphere of hydrogen at room temperature overnight. Further Pd-5% Barium sulphate (16.02 mg, 7.53 μmol) was added and the reaction mixture was stirred at room temperature under an atmosphere of hydrogen for 16 hours. The resulting mixture was filtered through Celite® eluting with EtOAc and the solvent was removed under reduced pressure. The crude material was adsorbed onto silica and purification by chromatography eluting with 0-100% EtOAc in iso-hexane afforded the title compound;
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09403810B2 |
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| Quelldatensatz | uspto-grants-2016_08 |
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| ORD ID | ord-e0eb9d9e3d6749e299366994d18a99ad |
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| Quellennotiz | uspto-grants-2016_08 |
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