3-Methylpyridine → 3-Pyridineacetonitrile

Participants

Reaction Steps

As the reactor there was used a quartz tube 1 meter long and 20 mm wide which was heated from the outside. There were fed into the tube separately from each other in homogeneous flow hourly 7.1 grams (0.12 mole) of cyanogen chloride and 42.8 grams (0.46 mole) of 3-methylpyridine) both of which were preheated to 550° C. The reaction temperature was 680° C. The reaction mixture was treated hourly with 1.2 liters of 5 percent aqueous sodium hydroxide solution in a gas washer directly post-connected to the reactor. The aqueous mixture which discharged from the gas washer was extracted hourly with 2 liters of dichloromethane. By distillation of the organic phase there were recovered the dichloromethane and the unreacted 3-methylpyridine. The pyridine-3-acetonitrile obtained had a boiling point of 101° to 109° C. at 1, 5 mbar. Its purity was 98 to 99%. The yield amounted to 10.4 grams, corresponding to 75% based on the cyanogen chloride added.

Provenance & Evidence