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喻魔风

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[求助] 2,5-二氯二苯甲酮的合成与应用

2,5-二氯二苯甲酮的合成与应用 要写综述找不到材料  急急急  求帮助

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[ Last edited by 喻魔风 on 2013-6-25 at 12:34 ]
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jsczlimin

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493070060: 金币+1, 鼓励交流,欢迎常来精化版! 2013-07-11 14:05:12
zhoupeng87: 应助指数+1 2013-07-12 08:22:42
对二氯苯1.5三氯化铝1.2苯甲酰氯1 。 滴加酰氯,吸收氯化氢,慢慢升温至150度至无氯化氢。到入5倍量水中。油层用甲醇重结晶。
2楼2013-07-11 13:43:26
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tangfh1973

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zhoupeng87: 金币+5, 欢迎交流 2013-07-30 08:01:08
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.
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3楼2013-07-29 10:54:26
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