Sodium Cyanide → 2-(2-Methylpyridin-3-yl)acetonitrile

HRID 889296

Reaktionsgleichung

Reaktionsgleichung von HRID 889296
Cl[CH2:2][C:3]1[C:4]([CH3:9])=[N:5][CH:6]=[CH:7][CH:8]=1.[C-:10]#[N:11].[Na+].[Cl-].[NH4+]>CN(C=O)C>[CH3:9][C:4]1[C:3]([CH2:2][C:10]#[N:11])=[CH:8][CH:7]=[CH:6][N:5]=1

Komponenten

5

Edukt 3

HCID 8929Sodium CyanideHCID 25517Ammonium ChlorideHCID 122437113-(Chloromethyl)-2-methylpyridine

Produkt 1

HCID 190992862-(2-Methylpyridin-3-yl)acetonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

970 mg (6.85 mmol) of the compound from Example 37A are initially introduced into 10 ml DMF, 336 mg (6.85 mmol) sodium cyanide are added and the mixture is stirred overnight at 45° C. The reaction mixture is introduced on to 75 ml saturated ammonium chloride solution and extracted several times with methylene chloride. The combined organic phases are dried over sodium sulfate, filtered and concentrated. The residue is purified by means of flash chromatography on silica gel (mobile phase: methylene chloride/methanol 20:1).

Aufarbeitung

  1. additionare added
  2. extractionextracted several times with methylene chloride
  3. dry with materialThe combined organic phases are dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue is purified by means of flash chromatography on silica gel (mobile phase: methylene chloride/methanol 20:1)

Quellen und Nachweise

ORD-Eintrag
ord-3b8056ed72f54a7daab4e4e314dd8c78
Quelldatensatz
uspto-grants-2012_08
Patentnummer
US08252817B2

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