Potassium Carbonate → HCID 54517635, compound

Participants

Reaction Steps

To a solution of 1-(4-amino-quinazoline-7-ylmethyl)-3-methyl-piperazine-2-one, EXAMPLE 80, (0.06 g, 0.2 mmol) in 2 mL of DMF is added 3-bromomethyl-7-chloroisoquinoline, EXAMPLE 11, 0.052 g, 0.20 mmol), and K2CO3 (0.08 g, 0.06 mmol). After 16 h, the reaction mixture is concentrated to dryness The crude product is purified by RP-HPLC eluting with a gradient of 5% CH3CN/H2O (0.1% TFA) to 50% CH3CN/H2O (0.1% TFA). The product fractions are lyophilized to give the title compound as a tristrisfluoroacetic acid salt (0.06 g, 0.08 mmol) as a white solid. 1H NMR (d6-DMSO, 300 MHz) δ9.79 (bs, 2H), 9.40 (s, 1H), 8.73 (s, 1H), 8.33 (d, 1H), 8.25 (s, 1H), 8.06 (s, 1H), 8.00 (d, 1H), 7.79 (d, 1H), 7.60 (m, 2H), 4.80 (AB, 2H), 4.72 (AB, 2H), 4.28 (m, 1H), 3.54 (m, 4H), 1.96 (d, 3H). MS (ion spray) 447, 449, (Cl pattern). Elemental analysis C28H25ClF6N6O6.3CF3CO2H.0.28H2O, cal C=45.38%, H=3.35%, N=10.58%; found C=45.38, H=3.35%, N=10.63%.

Provenance & Evidence