Iodine → HCID 86758968, compound

Participants

Reaction Steps

Iridium complex (1,5-cyclooctadiene bis(methyldiphenylphosphine)iridium hexafluorophosphate, 136 mg, 0.12 mmol) was suspended in tetrahydrofuran (5 mL), and activated by stirring under H2 flow. To this solution Compound 25 (940 mg, 1.16 mmol) dissolved in tetrahydrofuran (5 mL) was added, and the mixture was stirred at room temperature for 1 hour under argon gas flow. Iodine (588 mg), water (30 mL) and tetrahydrofuran (15 mL) were added thereto, and the mixture was further stirred at room temperature for 1.5 hours. The reaction mixture was diluted with chloroform, and washed successively with saturated sodium thiosulfate solution, saturated aqueous sodium hydrogencarbonate, and saturated brine. The chloroform layer was dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (toluene:acetone=6:1) to obtain Compound 26 (748 mg, 88.2%).

Provenance & Evidence