Hydrochloric Acid → HCID 178457929, compound

Participants

Reaction Steps

A solution of 278.5 mg of 3-[3-[5-fluoro-6-(4-methylperhydro-1,4-diazepin-1-yl)-1H-benzimidazol-2-yl]-1-(tetrahydropyran-2-yl)-1H-pyrazol-4-yl]-1,1-diisopropylurea in solution in 5.1 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 with, as eluent, a gradient of water/acetonitrile containing respectively 0.07% of trifluoroacetic acid. 15.2 mg of 3-{3-[5-fluoro-6-(4-methylperhydro-1,4-diazepin-1-yl)-1H-benzimidazol-2-yl]-1H-pyrazol-4-yl}-1,1-diisopropylurea are isolated in the form of a trifluoroacetate salt. 1H NMR (300 MHz, DMSO-d6, δ in ppm): 1.26 (d, J=7.0 Hz, 12H); 2.21 (broad m, 2H); 2.90 (s, 3H); from 3.14 to 3.68 (m, 8H); 3.90 (m, 2H); 7.16 (d, J=8.0 Hz, 1H); 7.48 (d, J=12.0 Hz, 1H); 7.98 (s, 1H). ES mass spectrum: m/z=457: MH+(base peak)—m/z=330 (MH−C7H13NO)+.

Provenance & Evidence