Hydrochloric Acid → HCID 53473321, compound

Participants

Reaction Steps

To a solution of (R)-6-(2-aminoethyl)-3-((S)-1-(2′,4′-difluorobiphenyl-4-yl)ethyl)-6-(4-fluoro-phenyl)-1,3-oxazinan-2-one (30 mg, 0.065 mmol) and urea (16 mg, 0.26 mmol) in H2O (3 mL) was added concentrated HCl (0.05 mL), and the mixture was refluxed overnight. The reaction mixture was crystallized by standing at rt. The precipitate was filtered and rinsed well with water to give 1-(2-((R)-3-((S)-1-(2′,4′-difluorobiphenyl-4-yl)ethyl)-6-(4-fluorophenyl)-2-oxo-1,3-oxazinan-6-yl)ethyl)urea (20 mg, 68%). LC-MS Method 3 tR=1.3, min, m/z=498; 1H NMR (CDCl3): 1.54-1.60 (d, 3H), 2.01-2.09 (m, 1H), 2.22-2.41 (m, 4H), 2.91-3.14 (m, 2H), 3.35-3.44 (m, 1H), 5.56-5.62 (s, 1H), 5.63-5.71 (m, 1H), 6.87-6.99 (m, 2H), 7.01-7.12 (m, 3H), 7.22-7.31 (m, 2H), 7.32-7.48 (m, 3H).

Provenance & Evidence