反应详情

2-Methoxyaniline (80 mg, 318 mmol) was added to a mixture of 3-amino-6-[4-[(4-methyl-1-piperazinyl)sulfonyl]phenyl]-2-pyrazinecarboxylic acid (80 mg, 212 mmol), O-(benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (82 mg, 255 mmol), 1-hydroxybenzotriazole hydrate (34 mg, 255 mmol) and N-ethyl-N,N-diisopropylamine (0.111 mL, 0.637 mmol) in N,N-dimethylformamide (2 mL). The reaction mixture was stirred for 13 h. The reaction was quenched with water (1 mL) and the solvent was evaporated. Purification by preparative HPLC (column: XTerra C8 19×300 mm, eluent: a acetonitrile/water, (20:80 to 80:20), gradient) followed by evaporation of the solvent gave a yellowish solid that was dissolved in methylene chloride (10 mL). HCl in diethyl ether (1 M, 2.5 mL) was added while stirring. Filtration and drying gave 12 mg (12% yield) of the title compound: MS (ESI) 483 m/z (M++1).

1. customThe reaction was quenched with water (1 mL)
2. customthe solvent was evaporated
3. customPurification by preparative HPLC (column
4. customXTerra C8 19×300 mm, eluent: a acetonitrile/water, (20:80 to 80:20), gradient) followed by evaporation of the solvent
5. customgave a yellowish solid
6. stirringwhile stirring
7. filtrationFiltration
8. customdrying