Hydrochloric Acid → HCID 178457930, compound

Participants

Reaction Steps

A solution of 600 mg of 3-[3-(5-fluoro-6-perhydro-1,4-oxazepin-4-yl-1H-benzimidazol-2-yl)-1-(tetrahydropyran-2-yl)-1H-pyrazol-4-yl]-1,1-diisopropylurea in solution in 5 mL of a 4N solution of hydrochloric acid in dioxane is stirred at 22° C. for 4 hours. After evaporation, the reaction crude is purified by preparative HPLC and then by preparative LC/MS, with, as eluent, a gradient of water, with acetonitrile, containing respectively 0.07% of trifluoroacetic acid. 48 mg of 3-[3-(5-fluoro-6-perhydro-1,4-oxazepin-4-yl-1H-benzimidazol-2-yl)-1H-pyrazol-4-yl]-1,1-diisopropylurea are obtained in the form of a brown solid. 1H NMR (400 MHz, DMSO-d6, δ in ppm): 1.35 (d, J=7.0 Hz, 12H); 1.98 (m, 2H); 3.33 (m, 4H); 3.78 (m, 4H); 4.06 (m, 2H); 7.08 (broad d J=8.0 Hz, 1H); 7.28 (broad d, J=12.0 Hz, 1H); 8.01 (s, 1H); 9.56 (s, 1H); 12.85 (broad m, 2H).

Provenance & Evidence