反应详情

1.99 g (4.73 mmol) of Compound 51 obtained in Example 51 was dissolved in 80 ml of dimethylformamide under argon atmosphere, 212 mg. of sodium hydride (60% oil disperison) and 0.60 ml of iodomethane were added and the mixture was stirred at room temperature for 1 hour. An aqueous saturated solution of ammonium chloride was added to the reaction solution, the precipitated crystals were collected by filtration and dissolved in ethanol, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (chloroform) to give 2.09 g of 5-amino-2-[4-[N-(tert-butoxycarbonyl)-N-methylamino]-3-fluorophenyl]-6,8-difluoro-4H-1-benzopyran-4-one.

1. filtrationthe precipitated crystals were collected by filtration
2. dissolutiondissolved in ethanol
3. distillationthe solvent was distilled off under reduced pressure
4. customThe residue was purified by silica gel column chromatography (chloroform)