Reacción #629933

Ecuación de reacción

ammonia

2-cyano-3-methyl pyridine

sulphuric acid

toluene

→

N-(1,1-dimethylethyl)-3-methyl-2-pyridine carboxamide

Disolventes

water

t-BuOH

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrois kept at 50°-55° C. during the work
2. 2
   OtroThe toluene phase is separated
3. 3
   Lavadothe combined toluene phases are washed with water
4. 4
   OtroRemoval of the toluene

Procedimiento

2-cyano-3-methyl pyridine (400 g) is suspended in t-BuOH (800 mL) and the mixture heated to 70° C. Concentrated sulphuric acid (400 mL) is added dropwise over 45 minutes. The reaction is complete after a further 30 minutes at 75° C. The mixture is then diluted with water (400 mL), charged with toluene (600 mL) and brought to pH 10 with concentrated aqueous ammonia. The temperature is kept at 50°-55° C. during the work up. The toluene phase is separated, the aqueous layer reextracted and the combined toluene phases are washed with water. Removal of the toluene yields an oil, N-(1,1-dimethylethyl)-3-methyl-2-pyridine carboxamide, from which solid product may crystallize. Product yield of 97% is determined by internal standard assay on gas chromatograph.

Fuente