反应详情

温度

120 °C

The piperazine from step A was combined with phenyl N-3-bromophenyl-N′-cyanocarbamimidate, from example 5, step A, (40 mg, 1.2 mmol) in isopropanol in a sealed tube. The reaction was heated to 120° C., monitored by LC/MS until no starting material remained, and then concentrated under vacuum. The residue was purified by prep HPLC (Sunfire C18 5u 30×100 mm, 10% to 100% B, gradient time=13 min, flow rate=45 ml/min, wavelength=220 nm, solvent A=10 mM aq. Ammonium acetate, solvent B=acetonitrile) to give (S)—N-(3-bromophenyl)-N′-cyano-2-isopropyl-4-(5-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)piperazine-1-carboximidamide (2.2 mg, 7%) as a white solid.

1. concentrationconcentrated under vacuum
2. customThe residue was purified by prep HPLC (Sunfire C18 5u 30×100 mm, 10% to 100% B, gradient time=13 min, flow rate=45 ml/min, wavelength=220 nm, solvent A=10 mM aq. Ammonium acetate, solvent B=acetonitrile)