Hydrochloric Acid → 5-cyano-3-methyl-pyridine-2-carboxylic acid [3-((R)-5-amino-3-difluoromethyl-3,6-dihydro-2H-[1,4]oxazin-3-yl)-4-fluoro-phenyl]-amide hydrochloride hydrate

Participants

Reaction Conditions

Reaction Steps

2.3 g of 5-cyano-3-methyl-pyridine-2-carboxylic acid [3-((R)-5-amino-3-difluoromethyl-3,6-dihydro-2H-[1,4]oxazin-3-yl)-4-fluoro-phenyl]-amide (5.702 mml) was put in a 4neck flask. In an Erlenmeyer flask 92 ml acetonitrile and 4.6 ml water were added. The mixture was shaken for a few seconds and 561.6 mg of HCl 37% (5.702 mmol) were added. The solution was shaken again for a few seconds and then it was added to the 4neck flask in portions. The mixture was stirred with a paddle and it was heated in a water bath up to 85° C. At 85° C. all the solid material was completely dissolved and a slightly yellow clear solution was obtained. The solution was left at rt to cool down with stirring. Precipitate appeared at 40° C. The suspension was let to stir overnight and it was filtered after 16 hours through a Büchner filter. The isolated material was dried in an oven at rt for 16 h and 1854.5 mg of a white powder was obtained.

Provenance & Evidence