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

HRID 1457884Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1457884
[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-b0f236273e7b40f68a5e199715e530a3
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05849768

Notizen zur Reaktion

Wird geladen…