1103738-29-9

1103738-26-6

1103738-29-9

Under nitrogen protection, 1 g of (2-chloro-5-iodophenyl)(4-ethoxyphenyl)methanone and 10.88 g of dichloromethane were added to a 100 mL reaction flask and heated to 30-40 °C. Subsequently 2.88 g of acetonitrile and 0.2 g of sodium borohydride were added and the reaction was stirred at 30-40 °C for 0.5 hours. Slowly 0.84 g of trimethylchlorosilane was added dropwise and the temperature was maintained at 30-40 °C for 4 hours of reaction. After that, 0.6 g of sodium borohydride and 2.52 g of trimethylchlorosilane were added and the reaction was continued at 30-40°C for 4 hours. The reaction solution was cooled to 0-5 °C, 2.2 g of boron trifluoride diethyl ether was added slowly dropwise, the temperature was controlled to be lower than 10 °C, and then the temperature was raised to 30-35 °C and maintained for 4 hours. Cooled again to 10-15 °C, added 0.6 g of sodium borohydride and 1.65 g of boron trifluoride diethyl ether, and heated to 30-35 °C for 4 hours. After the reaction was completed, cooled to 0-5 °C, 20 mL of dichloromethane was added, 20 mL of 12% sodium carbonate solution was added slowly dropwise, and stirring was continued for 20 minutes after the drop. The liquid was separated and the aqueous phase was extracted twice with 40 mL of dichloromethane. The organic phases were combined, washed with water once, dried with anhydrous sodium sulfate, filtered and concentrated under reduced pressure to obtain a light yellow oily crude product. The crude product was dissolved in 3mL of toluene, heated to 60°C, slowly added 12mL of methanol dropwise, cooled to -10°C and crystallized for 8 hours. Filtering, drying, to get 0.85g white solid product, yield 86%.