Reaktion #710482

ord-90bae05e2b3541eb987dc28d6e2c1646

Reaktionsgleichung

ClCc1ccc(Cl)nc1
2-chloro-5-chloromethyl pyridine
Nc1ccccn1
2-aminopyridine
Cl.N=c1ccccn1Cc1ccc(Cl)nc1
1-[(6-chloropyridin-3-yl)methyl]pyridin-2(1H)-imine hydrochloride
Ausbeute 86.9%

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONDMF was distilled off under reduced pressure, acetonitrile
  2. 2
    workup.ADDITIONwas added
  3. 3
    Sonstigeto precipitate a solid
  4. 4
    Sonstigethe solid was collected
  5. 5
    Waschenwashed well with acetonitrile
  6. 6
    Sonstigedried

Vorschrift

3.00 g (18.6 mmol) of 2-chloro-5-chloromethyl pyridine was dissolved in 20 ml of anhydrous DMF, 1.75 g (18.6 mmol) of 2-aminopyridine was added thereto, and the resulting mixture was stirred at 80° C. for 8 hours and at room temperature for 5 hours. After the reaction was completed, DMF was distilled off under reduced pressure, acetonitrile was added thereto to precipitate a solid, and the solid was collected, washed well with acetonitrile and then dried to obtain 2.07 g (yield 44%) of 1-[(6-chloropyridin-3-yl)methyl]pyridin-2(1H)-imine hydrochloride.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09301525B2uspto-grants-2016_04