反应详情

温度

80 °C

10 mL of concentrated sulfuric acid was added to 725 mg (1.44 mmol) of the above 2-[4-[N-acetyl-N-(3-dimethylaminopropyl)amino]-3-fluorophenyl]-6,8-difluoro-5-pentylamino-4H-1-benzopyran-4-one and the mixture was stirred at 80° C. for 20 minutes. The reaction solution was poured into ice water, the mixture was adjusted to pH 7 by addition of a 10N aqueous solution of sodium hydroxide thereto, and the precipitated crystals were collected by filtration. The crystals were purified by silica gel column chromatography (chloroform:methanol=20:1-9:1) and recrystallized from ethyl acetate/n-hexane to give 473 mg of Compound 127 (yield: 71%), which was converted to hydrochloride according to the conventional method.

1. filtrationthe precipitated crystals were collected by filtration
2. customThe crystals were purified by silica gel column chromatography (chloroform:methanol=20:1-9:1)
3. customrecrystallized from ethyl acetate/n-hexane