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[求助]
2，5-二氯二苯甲酮的合成與應(yīng)用
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2，5-二氯二苯甲酮的合成與應(yīng)用 要寫綜述找不到材料 急急急 求幫助 [ 發(fā)自手機(jī)版 http://www.gaoyang168.com/3g ] [ Last edited by 喻魔風(fēng) on 2013-6-25 at 12:34 ] |
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tangfh1973
鐵桿木蟲 (著名寫手)
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zhoupeng87: 金幣+5, 歡迎交流 2013-07-30 08:01:08
zhoupeng87: 金幣+5, 歡迎交流 2013-07-30 08:01:08
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2,5-Dichlorobenzophenone To a 22 L, three-necked flask fitted with a thermometer, mechanical stirrer and a Vigreux column connected to an aqueous NaOH scrubbing tower, was added 1,4-dichlorobenzene (3 Kg, 26.4 mol) and benzoyl chloride (2.6 Kg, 18.55 mol). The mixture was heated to 80° C. to give a homogeneous solution. Aluminum chloride (5.5 Kg, 41.25 mol) was added over 12 min. with stirring. (The molar ratio of reactants was 2.2:1.4:1.0 (AlCl3: Dichlorobenzene:Benzoyl Chloride)). The resulting mixture was heated to 140° C. over 60 min followed by heating to 175° C. over 30 min. Heating was stopped at 175° C. The mixture was allowed to cool to 80° C. over two hours and poured into a well stirred mixture of ice and water (ca. 25 L water and 15 Kg of ice) over 30 min. The organic solid was collected by filtration and dissolved in 7 L of toluene. The solution was washed with aqueous sodium bicarbonate and dried. Toluene was removed by distillation. Pure 2,5-dichlorobenzophenone was isolated in 80percent yield after recrystallization from hexane and toluene. Gas chromatography indicated an absolute yield of 97percent. |
3樓2013-07-29 10:54:26
2樓2013-07-11 13:43:26
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