Reaktion #1106

ord-ed5d30e63cae482aa9ed8a44a63361f9

Reaktionsgleichung

COc1c(Cl)ccnc1C
4-chloro-3-methoxy-2-methylpyridine
CC(C)(C)c1ccc(N)cc1
4-tert-butylaniline
[Na+].[OH-]
NaOH
COc1c(Nc2ccc(C(C)(C)C)cc2)ccnc1C
4-(4-tert-Butylanilino)-3-methoxy-2-methylpyridine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Extraktionthe product is extracted
  3. 3
    EinengenAfter concentrating
  4. 4
    workup.DISTILLATIONthe excess of amine is distilled off in vacuo
  5. 5
    Sonstigethe residue is crystallized

Vorschrift

7.9 g of 4-chloro-3-methoxy-2-methylpyridine and 22.4 g of 4-tert-butylaniline are heated at 120° C. for 8 hours in 20 g of phenol. After cooling, the mixture is poured into NaOH and the product is extracted using methylene chloride. After concentrating, the excess of amine is distilled off in vacuo and the residue is crystallized using hexane. 9.5 g=55%

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05723450uspto-grants-1998_03