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To a solution of <strong>[261723-32-4](3-bromo-2-fluorophenyl)methanol</strong> (5.0 g, 24 mmol) in tetrahydrofuran (50 mL) at 0 C under nitrogen was added sodium hydride ( 1.9 g, 49 mmol, 60 % w/w) in portions. The mixture was stirred at 0 C for 30 minutes, and iodomethane (17 g, 72 mmol) was added to the mixture. The reaction mixture was stirred at room temperature for 1.5 h, then quenched with ice-water (50 mL), stirred for 30 min. and extracted with ethyl acetate (3 chi 50 mL). The combined organic layers were washed with brine (2 chi 50 mL), dried over anhydrous sodium sulfate, concentrated in vacuo and purified by silica gel column chromatography [petroleum ether: ethyl acetate = 15: 1] to give compound B-261 (5.2 g, 94% yield) as a yellow oil.
With sodium hydride; In tetrahydrofuran; mineral oil; at 20℃;Cooling with ice;
To an ice-cold solution of Compound II (500 mg) in THF (5.0 mL) were added sodium hydride (160 mg, 55% contents) and methyl iodide (608 muL), and the resulting mixture was stirred at room temperature overnight. To the reaction mixture was added water, and the mixture was concentrated under reduced pressure. The residue was diluted with water, and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=4/1) to give Compound III (426 mg).
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