2-Aminopyridine → N-(5-pyrimidinylmethylene)-2-pyridinamine

HRID 515552Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 515552
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[N:8]1[CH:13]=[C:12]([CH:14]=O)[CH:11]=[N:10][CH:9]=1>C(Cl)(Cl)Cl>[N:8]1[CH:13]=[C:12]([CH:14]=[N:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=2)[CH:11]=[N:10][CH:9]=1

Komponenten

4

Edukt 2

HCID 104392-AminopyridineHCID 2761034Pyrimidine-5-carboxaldehyde

Produkt 1

HCID 68282155N-(5-pyrimidinylmethylene)-2-pyridinamineAusbeute 99,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel3×

Versuchsvorschrift

A solution of 2-aminopyridine (11.314 g, 120.3 mmol) and pyrimidine-5-carboxaldehyde (14.0 g, 129.6 mmol) in chloroform (300 mL) was stirred at room temperature for 15 min. The volatiles were then removed under reduced pressure (1 h at 75° C.) to yield a yellow solid. The crude solid was dissolved in chloroform (300 mL) and the solution was stirred for 15 min. The volatiles were then removed under reduced pressure (1 h at 75° C.) to yield a yellow solid. The crude solid was again dissolved in chloroform (300 mL), the solution was stirred for 15 min, and the volatiles were removed under reduced pressure (1 h at 85° C.) to yield a yellow solid. This solid was dried in a vacuum oven overnight at 80° C. to yield 22.090 g (99.8%) of the title compound.

Aufarbeitung

  1. customThe volatiles were then removed under reduced pressure (1 h at 75° C.)
  2. customto yield a yellow solid
  3. customThe volatiles were then removed under reduced pressure (1 h at 75° C.)
  4. customto yield a yellow solid
  5. stirringthe solution was stirred for 15 min
  6. customthe volatiles were removed under reduced pressure (1 h at 85° C.)
  7. customto yield a yellow solid
  8. customThis solid was dried in a vacuum oven overnight at 80° C.

Quellen und Nachweise

ORD-Eintrag
ord-8448ac91cd3e43139bff4f0665ee5357
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09108965B2

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