Iodine → HCID 14332264, compound

Participants

Reaction Steps

Under hydrogen gas atmosphere, a solution of Compound 12 (8.9 g, 16.7 mmol) in tetrahydrofuran (80 ml) was added to a solution of activated iridium complex (Ir(CoD)(PMePh2)2PF6, 287 mg, 0.34 mmol) in tetrahydrofuran (60 ml) at room temperature, and the mixture was stirred for 7 hours. Subsequently, water (100 ml) and iodine (8.5 g, 67.1 mmol) were added to the reaction mixture, and it was stirred for 15 hours. The reaction mixture was diluted with ethyl acetate, washed successively with saturated sodium thiosulfate solution, saturated aqueous sodium hydrogencarbonate, and saturated brine, and dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was recrystallized (ethanol/dichloromethane/diethyl ether) to obtain Compound 13 (7.4 g, 97%).

Provenance & Evidence