6-{2-[(Propan-2-yl)amino]propyl}pyridin-3-ol → 3-Pyridinol, 6-[2-[(1-methylethyl)amino]propyl]-, (2E)-2-butenedioate (1:1) (salt)

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Reaction Steps

To the suspension of 116 g of 2-(2-isopropylaminopropyl)-5-pyridinol and 310 ml of water, 65 g of fumaric acid are added while stirring at 70° under nitrogen. The resulting clear solution is stirred at 20° overnight, the precipitate formed filtered off and washed 3 times with 15 ml of cold water each. 873 g thereof (from several batches) are dissolved in 2,100 ml of water at 70°, the solution filtered hot and the filtrate stirred at room temperature under nitrogen for 2 days. The resulting suspension is filtered and the residue washed twice with 250 ml of cold water each, to yield the 2-(2-isopropylaminopropyl)-5-pyridinol monofumarate melting at 180°-183° with decomposition.

Provenance & Evidence