Hydrochloric Acid → 3-Amino-6-chloropyridine-2-carbonitrile

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Reaction Steps

Added 4 g (21.8 mmol) of 2-cyano-3-nitro-6-chloropyridine into concentrated hydrochloric acid (15.00 mL) and ethanol (45.00 mL), then the solution was stirred thoroughly. 4.27 g (76.3 mmol) of reduced iron powder was added in batches to the mixture under a speed that maintained a slight boiling in the flask. The mixture was heated under reflux for 30 min, poured into ice-water (650 mL), stirred, and filtered. Sufficient aether was added to the filter cake and the mixture was stirred thoroughly and filtered. The filtrate was dried with anhydrous magnesium sulfate. The filtrate was adjusted to alkaline with concentrated ammonia first, then filtered and extracted with ether for 3 times. The combined solution of the organic phase and ether solution was dried with anhydrous magnesium sulfate before combined, and then filtered and evaporated under reduced pressure to yield 2.92 g of yellow solid product with a recovery rate of 87.42%.

Provenance & Evidence