2,6-二异丙基-4-苯氧基苯基异硫氰酸酯的合成  被引量:4

Synthesis of 2 , 6-Diisopropyl-4-Phenoxyphenyl Isocyanate

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作  者:方永勤[1] 武安邦[1] 

机构地区:[1]常州大学设计研究院,江苏常州213164

出  处:《常州大学学报(自然科学版)》2012年第4期24-27,共4页Journal of Changzhou University:Natural Science Edition

摘  要:以2,6-二异丙基苯胺为原料,经溴化、Ullmann缩合、硫氰化得到2,6-二异丙基-4-苯氧基苯基异硫氰酸酯,并考察了反应条件对收率的影响。较优工艺为,溴化:-5℃,n(2,6-二异丙基苯胺)∶n(Br2)=1.00∶1.05;Ullmann缩合:155℃,8-羟基喹啉铜为催化剂,n(2,6-二异丙基-4-溴苯胺)∶n(苯酚)∶n(KOH)=1.0∶1.3∶1.2;硫氰化:70℃,n(BTC)∶n(硫代甲酸盐)=1.0∶3.0,3步总收率82.2%。产品结构经IR、1H NMR谱确认。2,6-Diisopropyl-4-phenoxyphenyl isocyanate was prepared by 2,6-diisopropylaniline via bromation,Ullmann condensation and thiocyanation reaction.The effects of reaction conditions were investigated,and the optimal conditions were as follows,bromation:at-5℃,n(2,6-diisopropylaniline)∶n(Br 2) =1.00∶1.05;Ullmann condensation:at 155℃,copper 8-hydroxyquinoline as catalyst,n(2,6-diisopropyl-4-bromo aniline)∶n(phenol)∶n(KOH) =1.0∶1.3∶1.2;thiocyanation:at 70℃,n(BTC)∶n(dithiocarbamate) =1.0∶3.0,total yield after three steps was 82.2%.All compounds obtained were identified by IR and 1 H NMR.

关 键 词:2 6-二异丙基苯胺 2 6-二异丙基-4-苯氧基苯基异硫氰酸酯 二(三氯甲基)碳酸酯 ULLMANN反应 

分 类 号:TQ454.2[化学工程—农药化工]

 

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