Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | 2-Propylpyridine 1-oxide | HCID 88616 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Lösungsmittel | Acetic Anhydride | HCID 7918 | — |
| Produkt | 2-Propionylpyridine | HCID 520574 | — |
Reaktionsschritte
19 g of 2-propylpyridine-N-oxide were dissolved in 40 ml of glacial acetic acid/40 ml of acetic anhydride and stirred for 6 hours at 85° C. and 12 hours at ambient temperature. Excess anhydride was decomposed with H2O, the solution was neutralized with Na2CO3 and extracted with diethyl ether. After rotating in the ether phase, 12 g of 2-(1-acetoxypropyl)-pyridine remained. This product was dissolved in 120 ml of methanol (70%), mixed with 4 g of NaOH and refluxed for 6 hours. After rotating out the methanol mixing took place with water, extraction with diethyl ether and the organic phase was rotated in. 5.4 g of 2-(1-hydroxypropyl)-pyridine were left. 0.5 g of this substance was refluxed for 2 hours with 1 g of MnO2 and 30 ml of dichloromethane. After filtering off the MnO2, rotation in took place to dryness. 0.3 g of ethyl-2-pyridylketone was obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04997835 |
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| Quelldatensatz | uspto-grants-1991_03 |
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| ORD ID | ord-36bc9066493e4e6993f1129948a444ca |
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| Quellennotiz | uspto-grants-1991_03 |
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