反应详情

The compound (150 g, 335 mmol) obtained in Step 3 was dissolved in dimethylformamide (500 ml), imidazole (30 g, 0.436 mmol) and tert-butyldimethylsilyl chloride (56 g, 369 mmol) were added, and the mixture was stirred at room temperature for 1.5 hr. Water was added to the reaction mixture and extracted with ethyl acetate. The organic layer was washed successively with water, saturated aqueous ammonium chloride solution and saturated brine, and dried over sodium sulfate. The organic layer was filtered and the filtrate was concentrated under reduced pressure, and the obtained residue was purified by silica gel chromatography (ethyl acetate:hexane=1:3 to 1:2) to give 1-((S)-1-tert-butyldimethylsilyloxymethyl-2-methylpropyl)-7-fluoro-6-iodo-4-oxo-1,4-dihydroquinoline-3-carboxylic acid ethyl ester (173 g, yield 92%) as a colorless amorphous form.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed successively with water, saturated aqueous ammonium chloride solution and saturated brine
3. dry with materialdried over sodium sulfate
4. filtrationThe organic layer was filtered
5. concentrationthe filtrate was concentrated under reduced pressure
6. customthe obtained residue was purified by silica gel chromatography (ethyl acetate:hexane=1:3 to 1:2)