HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 1750743Erstellt: 25. Oktober 2026
Potassium Carbonate → Ethyl 4-(1,4-dioxa-8-azaspiro[4.5]decan-8-yl)benzoate
https://huagongshe.com/reaction/1750743
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 1,4-Dioxa-8-azaspiro(4.5)decane | HCID 67435 | — |
| Edukt | Benzoic acid, 4-fluoro-, ethyl ester | HCID 67976 | — |
| Lösungsmittel | Dimethylacetamide | HCID 31374 | — |
| Produkt | Ethyl 4-(1,4-dioxa-8-azaspiro[4.5]decan-8-yl)benzoate | HCID 12717439 | — |
Reaktionsschritte
Ethyl 4-fluorobenzoate (36.16 g, 215 mmol), 1,4-dioxa-8-azaspiro[4.5]decane (35.40 g, 247 mmol), and potassium carbonate (29.72 g, 215 mmol) were added to N,N-dimethylacetamide (500 mL) and heated to 100° C. for 16 hours. The solution was cooled, filtered, added to 2M HCl and extracted with 50% ethyl acetate (in hexanes). The organics were washed with water, brine, and dried on anhydrous sodium sulfate. The solution was concentrated and purified by flash column chromatography on silica gel with 20% ethyl acetate (in hexanes) increasing to 30% ethyl acetate (in hexanes).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09156856B2 |
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| Quelldatensatz | uspto-grants-2015_10 |
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| ORD ID | ord-7ec3b6423c08468fa344524c02d3faba |
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| Quellennotiz | uspto-grants-2015_10 |
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