Hydrochloric Acid → HCID 18322728, compound

Participants

Reaction Steps

232 g (0.66 mole) of ethyl β-[[2-[[(1,1-dimethylethoxy)carbonyl]amino]-1-oxoethyl]amino]-pyridine-3-propanoate (from Step C) was dissolved in 1 liter of warm dioxane. After cooling to room temperature, 1.6 liters of 4M HCl in dioxane (Aldrich) was slowly added. A white precipitate formed after several minutes and then turned to a thick goo. After 2 hours, the solvent was decanted off. Ether was slurried and decanted several times until a white solid resulted. This was dried under vacuum to yield 224.2 g of ethyl β-[(2-amino-1-oxoethyl]amino]pyridine-3-propanoate, bis(hydrochloride) salt as a white hygroscopic solid.

Provenance & Evidence