反应详情

In a 3-liter four-necked flask equipped with a stirring device, a thermometer, a condenser and a nitrogen substituting device, 34.39 g of 1,4-bis(4-(4-nitrobenzoyl)phenylmethyl) benzene was dissolved in 1000 milliliters of dichloromethane, and a solution of 37.8 g of titanium tetrachloride in 50 milliliters of dichloromethane was added dropwise for 1 hour with ice cooling. Subsequently, a solution of 41.46 g of triethylsilane in 50 milliliters of dichloromethane was added for 1 hour. 30 minutes after the end of the dropwise addition, stirring was carried out for 7 hours with ice cooling. After the end of the reaction was confirmed by a liquid chromatography, the reaction solution was neutralized with an aqueous solution of sodium carbonate and then washed with water. After removing off dichloromethane by a rotary evaporator, the solution was dissolved in chloroform, treated with an alumina column, and removed off the solvent from the solute. By recrystallizing the concentrate from an ethyl acetate solvent, 26.48 g of 1,4-bis(4-(4-nitrophenylmethyl)phenylmethyl)benzene was obtained as crystals.

1. customIn a 3-liter four-necked flask equipped with a stirring device
2. addition30 minutes after the end of the dropwise addition
3. washwashed with water
4. customAfter removing off dichloromethane
5. customby a rotary evaporator
6. dissolutionthe solution was dissolved in chloroform
7. additiontreated with an alumina column
8. customremoved off the solvent from the solute
9. customBy recrystallizing the
10. concentrationconcentrate from an ethyl acetate solvent