Dichloromethane → HCID 86661703, compound

Participants

Reaction Steps

To a round bottom flask 4-{4-[7-(4-Methanesulfonyl-phenyl)-pyrrolo[2,1-f][1,2,4]-triazin-2ylamino)-phenyl}-piperidine-1-carboxylic acid tert butyl ester (7-% pure, 0.762 g, 0.00135 mol) and 3.0 M Trifluoroacetic acid in DCM (10 mL, 0.030 mol) were added. The mixture was stirred at room temperature for 1 h then the solvent was removed by rotary evaporation. The crude product was purified via HPLC reverse phase chromatography with 0.1% TFA in Water and 0.1% TFA in ACN. The collected fractions were lyophilized to give [7-(4-Methanesulfonyl-phenyl)-pyrrolo[2,1-f][1,2,4]triazin-2-yl]-(4-piperidin-4-yl-phenyl)-amine; compound with trifluoro-acetic acid as a yellow fluffy solid (0.06 g, 10%). LCMS (E/I+) 448.1 (M+H). NMR 1H (CDCl3/DSMO-d6)-9.97 (s, 1H), 9.50 (s, 1H), 8.41 (d, 2H, J=8.52 Hz), 8.20 (s, 1H), 8.02 (d, 2H, J=8.51 Hz), 7.67 (d, 2H, J=8.67 Hz), 7.20 (d, 2H, J=7.6 Hz), 7.11 (d, 1H, J=4.90 Hz), 6.88 (d, 1H, J=4.88 Hz), 3.54 (d, 2H, J=12.06 Hz), 3.14 (s, 3H), 3.02 (m, 3H), 2.59 (m, 2H), 2.05 (m, 4H).

Provenance & Evidence