Nitric Acid → HCID 66665493, compound

Participants

Reaction Steps

To a solution of (R)-5-difluoromethyl-5-(2-fluoro-phenyl)-5,6-dihydro-2H-[1,4]oxazin-3-ylamine sulphate (127.2 g, 371.6 mmol) in conc. H2SO4 (380 mL) was added at 5-15° C. HNO3 (25.8 g, 408.8 mmol). After addition, the reaction mixture was added slowly to 12% NH3 water solution (2.6 L) at 10-20° C. The resulted suspension (pH˜8) was filtered to provide the title compound as a yellow solid: ESIMS: 290; [(M+H)+]; 1H NMR (400 MHz, CDCl3): δ 8.89 (m, 1H), 8.14 (m, 1H), 7.18 (dd, 1H), 6.10 (t, 1H), 5.65 (br s, 2H), 4.57 (dd, 1H), 4.13 (dd, 2H), 3.88 (m, 1H).

Provenance & Evidence