Hydrochloric Acid → HCID 23506216, Verbindung
Reaktionsgleichung
COC[O:4][C:5]1[CH:6]=[N:7][CH:8]=[CH:9][C:10]=1[CH2:11][CH2:12][CH2:13][OH:14].Cl>C(O)C>[OH:4][C:5]1[CH:6]=[N:7][CH:8]=[CH:9][C:10]=1[CH2:11][CH2:12][CH2:13][OH:14]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
3-(3-Methoxymethoxypyridin-4-yl)-1-propanol (3.67 g, 18.6 mmol) obtained in Example 2 is dissolved in ethanol (100 ml), and thereto is added a 15% aqueous hydrochloric acid solution (20 ml), and the mixture is heated under reflux for 30 minutes. The reaction solution is concentrated under reduced pressure, and the residue is purified by silica gel column chromatography (eluent: hexane/ethyl acetate), and further recrystallized from diethyl ether to give the title compound (2.08 g) as colorless crystals, m.p. 123-126° C.
Aufarbeitung
- temperaturethe mixture is heated
- temperatureunder reflux for 30 minutes
- concentrationThe reaction solution is concentrated under reduced pressure
- customthe residue is purified by silica gel column chromatography (eluent: hexane/ethyl acetate)
- customfurther recrystallized from diethyl ether
Quellen und Nachweise
- ORD-Eintrag
- ord-706c046adfdc4b8ab13cbe9712942833
- Quelldatensatz
- uspto-grants-2003_04
- Patentnummer
- US06555557B1
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