Methylamine → 2-(Methylamino)pyridine-4-carbonitrile

HRID 887636Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 887636
Cl[C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][N:9]=1)[C:5]#[N:6].[CH3:10][NH2:11].C([O-])(O)=O.[Na+]>N1C=CC=CC=1.C1COCC1>[CH3:10][NH:11][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][N:9]=1)[C:5]#[N:6]

Komponenten

6

Edukt 3

HCID 6329MethylamineHCID 516892Sodium BicarbonateHCID 5686382-Chloro-4-cyanopyridine

Produkt 1

HCID 219614802-(Methylamino)pyridine-4-carbonitrile

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

To a solution of 2-chloroisonicotinonitrile (22.0 g, 159 mmole) in pyridine (500 mL) was added methylamine in THF (2N, 160 mL), and NaHCO3 (54 g). The mixture was heated to 120° C. in a sealed vessel for 40 h. After cooled to RT, the mixture was filtered and the filter cake was washed with CH2Cl2. The combined filtrated was concentrated in vacuo to give a yellow solid (21 g) as the desired compound.

Aufarbeitung

  1. temperatureAfter cooled to RT
  2. filtrationthe mixture was filtered
  3. washthe filter cake was washed with CH2Cl2
  4. filtrationThe combined filtrated
  5. concentrationwas concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-dc279dcae4604efeabf4d69733ae5730
Quelldatensatz
uspto-grants-2012_08
Patentnummer
US08247430B2

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