反应详情

After adding 0.056 ml of triethylamine, 0.0015 g of 4-dimethylaminopyridine and 71 mg of di-t-butyl dicarbonate to a solution of 0.068 g of 5-{3-[(4-carbamimidoylphenylamino)-(2-fluoro-4,5-dimethoxyphenyl)methyl]-5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl}-1H-pyrazole-4-carboxylic acid ethyl ester acetate in 4 ml of acetonitrile, the mixture was stirred at room temperature for 15 minutes. The solvent was removed under reduced pressure, and then 1 ml of methanol and 1 ml of a 5N aqueous solution of sodium hydroxide were added and the mixture was further stirred at room temperature for 6 hours. Next, 2 ml of acetic acid, 1 ml of water and 1 ml of methanol were added to the reaction mixture, which was then stirred and heated at 50° C. for 15 hours. After cooling, purification was performed by reverse-phase high performance liquid chromatography (acetonitrile-water, 0.1% acetic acid) to give 0.034 g of the title compound.

1. customThe solvent was removed under reduced pressure
2. addition1 ml of methanol and 1 ml of a 5N aqueous solution of sodium hydroxide were added
3. stirringthe mixture was further stirred at room temperature for 6 hours
4. additionNext, 2 ml of acetic acid, 1 ml of water and 1 ml of methanol were added to the reaction mixture, which
5. stirringwas then stirred
6. temperatureheated at 50° C. for 15 hours
7. temperatureAfter cooling
8. custompurification