反应详情

The compound (22 g, 48 mmol) obtained in Step 3 was dissolved in dimethylformamide (60 ml), imidazole (3.9 g, 57.7 mmol) and tert-butyldimethylsilyl chloride (8.0 g, 53.0 mmol) were added, and the mixture was stirred at room temperature for 1.5 hr. The reaction mixture was concentrated under reduced pressure, and the obtained residue was dissolved in ethyl acetate (200 ml), washed successively with water (twice) and saturated brine, and dried over sodium sulfate. The mixture was filtered and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel chromatography (ethyl acetate:hexane=3:7 to 4:6) to give 1-((S)-1-tert-butyldimethylsilyloxymethyl-2-methylpropyl)-7-fluoro-6-iodo-4-oxo-1,4-dihydroquinoline-3-carboxylic acid ethyl ester (25 g, yield 92%) as a white wax.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. dissolutionthe obtained residue was dissolved in ethyl acetate (200 ml)
3. washwashed successively with water (twice) and saturated brine
4. dry with materialdried over sodium sulfate
5. filtrationThe mixture was filtered
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe obtained residue was purified by silica gel chromatography (ethyl acetate:hexane=3:7 to 4:6)