Sodium Iodide → HCID 86721401, compound

Participants

Reaction Steps

[step 4] Sodium iodide (4.63 g, 30.9 mmol) was suspended in a mixed solution of dichloromethane (15 mL)-acetone (15 mL), dichlorodimethylsilane (1.84 mL, 15.4 mmol) was added under ice-cooling, and the mixture was stirred for 15 min. Under ice-cooling, a solution (15 mL) of (E)-2-{8-[(8-chloro-2-cyclopropylimidazo[1,2-a]pyridin-3-yl)(hydroxy)methyl]-3-fluorodibenzo[b,e]oxepin-11(6H)-ylidene}propanenitrile (1.5 g, 3.09 mmol) obtained in step 3 in dichloromethane was added, and the mixture was stirred at room temperature for 30 min. To the mixture were added 10% aqueous sodium thiosulfate solution (50 mL) and saturated aqueous sodium hydrogen carbonate solution (100 mL), and the mixture was extracted 3 times with ethyl acetate. The combined organic layers were dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. To the obtained residue was added isopropylalcohol (15 mL)-diisopropyl ether (15 mL), and the precipitated crystals were collected by suction filtration to give the title compound (1.4 g, 97%).

Provenance & Evidence