Chloroform → HCID 22921204, compound

Participants

Reaction Steps

In a 1-liter four-necked flask equipped with a stirring device, a thermometer, a condenser and a nitrogen substituting device, 17.7 g of 1,1-bis(4-(4-(4-nitrobenzoyl)phenylmethyl) phenyl)methane was dissolved in 150 milliliters of dichloromethane, 14.5 g of triethylsilane and 20.7 g of boron trifluoride ethyl ether complex were added, and they were stirred for 20 hours at reflux of dichloroethane. After the end of the reaction was confirmed by a liquid chromatography, the reaction solution was cooled to room temperature, poured in 100 milliliters of ice water, and then 150 milliliters of chloroform was added for extraction. Thereafter, the solution was washed with a 6N-HCl aqueous solution of from 50° to 55° C., an aqueous solution of sodium hydrogencarbonate, brine and water, removed off chloroform and dichloroethane by a rotary evaporator, and then recrystallized from a chloroform solvent, to obtain 16.4 g of 1,1-bis(4-(4-(4-nitrophenylmethyl)phenylmethyl)phenyl)methane as crystals.

Provenance & Evidence