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Ethanol → 2-Hydroxymethyl-4-(3-methoxypropoxy)pyridine

HRID 727919
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 727919
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][N+:10]([O-])=[C:9]([CH3:14])[CH:8]=1.C([OH:17])C>C(OC(=O)C)(=O)C>[OH:17][CH2:14][C:9]1[CH:8]=[C:7]([O:6][CH2:5][CH2:4][CH2:3][O:2][CH3:1])[CH:12]=[CH:11][N:10]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 702EthanolHCID 151662164-(3-Methoxypropoxy)-2-methylpyridine 1-oxide

Produkt 1

HCID 151662262-Hydroxymethyl-4-(3-methoxypropoxy)pyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7918Acetic AnhydrideLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

4.05 g (0.02 mol) of 4-methoxypropoxy-2-methylpyridine 1-oxide was dissolved in 50 ml of acetic anhydride to obtain a solution. This solution was stirred at 90° C. for 0.5 hour and cooled, followed by the addition of ethanol. The obtained mixture was concentrated under a reduced pressure, followed by the addition of 150 ml of 1N hydrochloric acid. The obtained mixture was stirred at 100° C. for one hour, cooled, neutralized with sodium hydrogencarbonate and extracted with chloroform. The extract was dried over magnesium sulfate and filtered. The filtrate was distilled to remove the solvent. Thus, 3.64 g of the title compound was obtained as a crude product.

Aufarbeitung

  1. customto obtain a solution
  2. temperaturecooled
  3. concentrationThe obtained mixture was concentrated under a reduced pressure
  4. additionfollowed by the addition of 150 ml of 1N hydrochloric acid
  5. stirringThe obtained mixture was stirred at 100° C. for one hour
  6. temperaturecooled
  7. extractionextracted with chloroform
  8. dry with materialThe extract was dried over magnesium sulfate
  9. filtrationfiltered
  10. distillationThe filtrate was distilled
  11. customto remove the solvent

Quellen und Nachweise

ORD-Eintrag
ord-1cf69032d2624c82ae93b2cb2e4e231d
Quelldatensatz
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05045552

Notizen zur Reaktion

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