Methylamine → 6-Bromo-N-methyl-3-pyridinemethanamine

HRID 2187217Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2187217
[CH3:1][NH2:2].[Br:3][C:4]1[N:9]=[CH:8][C:7]([CH2:10]Br)=[CH:6][CH:5]=1>CC#N>[Br:3][C:4]1[N:9]=[CH:8][C:7]([CH2:10][NH:2][CH3:1])=[CH:6][CH:5]=1

Komponenten

4

Edukt 2

HCID 6329MethylamineHCID 64246602-Bromo-5-bromomethylpyridine

Produkt 1

HCID 224503166-Bromo-N-methyl-3-pyridinemethanamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a mixture of 12.3 g of 40% aqueous methylamine solution and 40 ml of CH3CN was added 8.0 g of crude (6-bromo-3-pyridyl)methyl bromide with stirring. The mixture was further stirred at room temperature for 30 minutes. The reaction mixture thus obtained was concentrated and the residue was diluted with toluene and subjected to azeotropic distillation to remove the water. Then, the soluble fraction was extracted with Et2O. The Et2O layer was dried over MgSO4 and concentrated to recover 4.4 g of the title compound as a yellow oil.

Aufarbeitung

  1. stirringThe mixture was further stirred at room temperature for 30 minutes
  2. customThe reaction mixture thus obtained
  3. concentrationwas concentrated
  4. additionthe residue was diluted with toluene
  5. distillationsubjected to azeotropic distillation
  6. customto remove the water
  7. extractionThen, the soluble fraction was extracted with Et2O
  8. dry with materialThe Et2O layer was dried over MgSO4
  9. concentrationconcentrated
  10. customto recover 4.4 g of the title compound as a yellow oil

Quellen und Nachweise

ORD-Eintrag
ord-293f7a85930947f791838f1470ec6696
Quelldatensatz
uspto-grants-2002_06
Patentnummer
US06407248B1

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