Ammonium Chloride → α,3-Dimethyl-4-pyridinemethanol

HRID 2092046Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2092046
[CH3:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]=[O:9].[CH3:10][Mg]Br.[Cl-].[NH4+]>O1CCCC1>[CH3:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]([OH:9])[CH3:10]

Komponenten

5

Edukt 3

HCID 25517Ammonium ChlorideHCID 15018803-Methyl-4-pyridinecarboxaldehydeHCID 178418573HCID 178418573, Verbindung

Produkt 1

HCID 59574200α,3-Dimethyl-4-pyridinemethanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

3-Methylpyridine-4-carbaldehyde (310.6 mg, 1.00 mmol) in tetrahydrofuran (6 mL) was mixed with methylmagnesium bromide (0.98 M in tetrahydrofuran, 4.74 mL, 4.65 mmol) under −78° C., and the mixture was warmed slowly to room temperature for 16 hours with stirring. After completion of the reaction, the reaction solution was mixed with saturated aqueous ammonium chloride and extracted with ethyl acetate, and the organic layer was dried over anhydrous sodium sulfate and evaporated under reduced pressure. The resulting crude reaction product containing the desired product was used for the next step (310.6 mg).

Aufarbeitung

  1. customAfter completion of the reaction
  2. extractionextracted with ethyl acetate
  3. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  4. customevaporated under reduced pressure
  5. customThe resulting crude reaction product

Quellen und Nachweise

ORD-Eintrag
ord-7bd446a8fcfb47f48736ffce306ac101
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08440666B2

Notizen zur Reaktion

Wird geladen…