Acetonitrile → HCID 14209973, compound

Participants

Reaction Conditions

Reaction Steps

160.0 g (0.58 mol) of the 2-amino-5-ethyl-N-(2-chloropyridin-3-yl)benzamide obtained were dissolved in 256 ml of sulpholane and heated to 170° C. with stirring for 20 minutes. The mixture was left to cool, stirred with 1 liter of acetonitrile, the resulting crystal slurry was suction filtered and washed successively with 50 ml acetonitrile and 100 ml conc. ammonia. It was recrystallised from hot 70% acetic acid and after drying in a circulating air dryer 114.0 g (48% of theory) of pale yellow crystals were obtained, m.p. 232°-234° C., RF 0.78 (Macherey-Nagel, PolygramRSIL G/UV254, pre-coated plastic sheets for TLC, eluant: dichloromethane/ethyl acetate 1/1 v/v).

Provenance & Evidence