1,4-二苯甲酰丁烷

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a 2-liter three-necked flask equipped with a stirring device and a nitrogen substituting device, 5 g of a Pd-C catalyst (a 5% product, containing 55.9% of water) and a solution of 100.9 g of 1,6-diphenylhexane-1,6-dione in 400 milliliters of tetrahydrofuran and 400 milliliters of denatured ethanol as well as 5 milliliters of 6N-hydrochloric acid were introduced, stirred at a normal pressure and contacted with hydrogen gas. After absorption of hydrogen was stopped, the catalyst was filtered off and the solution was concentrated. The concentrate was dissolved in ethyl acetate, washed with a dilute aqueous solution of sodium hydrogencarbonate and water, and thereafter dried with anhydrous sodium sulfate. After removing off the solvent by a rotary evaporator, a distillation under a decreased pressure was carried out, to obtain 85.3 g of 1,6-diphenylhexane as colorless liquid. In a 2-liter three-necked flask equipped with a stirring device were introduced After absorption of hydrogen the catalyst was filtered off the solution was concentrated The concentrate was dissolved in ethyl acetate washed with a dilute aqueous solution of sodium hydrogencarbonate and water dried with anhydrous sodium sulfate After removing off the solvent by a rotary evaporator a distillation under a decreased pressure

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a 2-liter three-necked flask equipped with a stirring device, a thermometer and a nitrogen substituting device, 700 milliliters of benzene was introduced and 177.0 g of aluminum chloride was added with ice cooling. Then, a solution of 101.6 g of adipoyl chloride in 300 milliliters of benzene was added dropwise for 35 minutes. After stirring for one day and one night with warming back to the room temperature, the solution was poured in 3 liters of ice water containing dilute hydrochloric acid, and extracted with 2.5 liters of toluene. Thereafter, the solution was washed with a 0.5N aqueous solution of sodium hydroxide and water, and then dried with anhydrous magnesium sulfate. After removing off the solvent by a rotary evaporator, 128.4 g of 1,6-diphenylhexane-1,6-dione was obtained as crystals by recrystallizing the obtained crystals from ethyl acetate. In a 2-liter three-necked flask equipped with a stirring device extracted with 2.5 liters of toluene Thereafter, the solution was washed with a 0.5N aqueous solution of sodium hydroxide and water dried with anhydrous magnesium sulfate After removing off the solvent by a rotary evaporator