4-chloro-6-methylfuro[3,2-c]pyridine → HCID 14005231, Verbindung
Reaktionsgleichung
Cl[C:2]1[C:7]2[CH:8]=[CH:9][O:10][C:6]=2[CH:5]=[C:4]([CH3:11])[N:3]=1>C(O)(=O)C.[Zn]>[CH3:11][C:4]1[N:3]=[CH:2][C:7]2[CH:8]=[CH:9][O:10][C:6]=2[CH:5]=1Komponenten
4
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 110 °C
Versuchsvorschrift
To a solution of 4-chloro-6-methylfuro[3,2-c]pyridine (12.98 g, 0.0776 mol) in glacial acetic acid (160 ml) under a nitrogen atmosphere was added zinc powder (7.0 g, 0.107 mol.). This mixture was heated at 110° C. for 2.5 hours and then filtered hot to remove zinc. The acetic acid solution was evaporated and the residue dissolved in water and made strongly basic by addition of sodium hydroxide. The zinc salts were filtered and washed thoroughly with methylene chloride. The aqueous filtrate was extracted with methylene chloride and the combined washings were dried over anhydrous sodium sulfate, filtered through a charcoal pad and the solvent evaporated to give 9.5 g (87% yield) of pure product, mp: 55°-56° C.
Aufarbeitung
- filtrationfiltered hot
- customto remove zinc
- customThe acetic acid solution was evaporated
- dissolutionthe residue dissolved in water
- additionmade strongly basic by addition of sodium hydroxide
- filtrationThe zinc salts were filtered
- washwashed thoroughly with methylene chloride
- extractionThe aqueous filtrate was extracted with methylene chloride
- dry with materialthe combined washings were dried over anhydrous sodium sulfate
- filtrationfiltered through a charcoal pad
- customthe solvent evaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-5004f29f6d914e57a7fb592358047ce4
- Quelldatensatz
- uspto-grants-1989_02
- Patentnummer
- US04808595
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