Water → HCID 66672506, compound

Participants

Reaction Conditions

Reaction Steps

1.8 g of 2-cyano-3,5-difluoropyridine, 1.375 g of 2-(2-aminoethyl)pyridine and 3.552 g of potassium carbonate in 27 ml of dimethyl sulphoxide are introduced into a 20 ml microwave tube reactor by means of three successive identical operations. The mixture is then heated in a microwave for 1 hour at 115° C. The reaction medium is run into 100 ml of water and 200 ml of ethyl acetate. The aqueous phase is re-extracted twice with 250 ml of ethyl acetate. The combined organic phases are washed with water and then with a saturated aqueous solution of sodium chloride, dried over sodium sulphate and concentrated under reduced pressure. After purification by flash chromatography on 200 g of silica gel, elution being carried out with a mixture of ethyl acetate and cyclohexane (50/50 by volume), and the first eluted product being recovered, 768 mg of 2-cyano-5-fluoro-3-(2-hydroxy-2-methylpropylamino)pyridine are thus obtained in the form of a beige powder, the characteristic of which is the following:

Provenance & Evidence