Methyl iodide → 3-Methoxy-1-methylpyridin-2-one

HRID 1076826

Reaktionsgleichung

Reaktionsgleichung von HRID 1076826
[CH3:1][O:2][C:3]1[C:4](=[O:9])[NH:5][CH:6]=[CH:7][CH:8]=1.[OH-].[K+].[CH3:12]I>CO>[CH3:12][N:5]1[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[C:4]1=[O:9]

Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 14797Potassium HydroxideHCID 887313-Methoxy-2-pyridone

Produkt 1

HCID 5870243-Methoxy-1-methylpyridin-2-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 3-methoxy-2(1H)-pyridone (25 g., 0.2 moles), potassium hydroxide (16 g., 0.24 moles) and methyl iodide (45.4 g., 0.32 moles) in 400 ml. methanol is heated at reflux for 5 hours. The methanol is removed under reduced pressure leaving a solid redidue which is extracted with methylene chloride. The methylene chloride extracts are washed with water, a saturated salt solution, and dried over sodium sulfate. Evaporation of the dried extracts, under reduced pressure, affords 1-methyl-3-methoxy-2(1H)-pyridone as a colorless oil which solidifies on standing (26.2 g., 94%). The pyridone is very hygroscopic and rapidly liquifies on exposure to air.

Aufarbeitung

  1. temperatureat reflux for 5 hours
  2. customThe methanol is removed under reduced pressure
  3. customleaving a solid redidue which
  4. extractionis extracted with methylene chloride
  5. washThe methylene chloride extracts are washed with water
  6. dry with materiala saturated salt solution, and dried over sodium sulfate
  7. customEvaporation of the dried extracts

Quellen und Nachweise

ORD-Eintrag
ord-14fbee2fa7ed4ca0bea4dcb2924b3026
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03957997

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