反应详情

The compound (260 mg) obtained in Step 1 of this Reference Example was dissolved in toluene (10 mL) and methylene chloride (1 mL). To the solution, a solution of sodium bicarbonate (210 mg, 2.50 mmol) in water (8 mL), iodine (370 mg), and 2,2,6,6-tetramethyl-1-piperidinyloxy (15 mg) were added in this order, and the mixture was stirred at room temperature for 12 hours. To the reaction solution, saturated aqueous sodium thiosulfate was added, and organic matter was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered, and the solvent was distilled off under reduced pressure to obtain a crude product. This crude product was purified by silica gel column chromatography (eluting solvent: hexane/ethyl acetate=2/1-1/1) to obtain the title compound (258 mg).

1. extractionorganic matter was extracted with ethyl acetate
2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
3. filtrationfiltered
4. distillationthe solvent was distilled off under reduced pressure
5. customto obtain a crude product
6. customThis crude product was purified by silica gel column chromatography (eluting solvent: hexane/ethyl acetate=2/1-1/1)