检索规则说明:AND代表“并且”;OR代表“或者”;NOT代表“不包含”;(注意必须大写,运算符两边需空一格)
检 索 范 例 :范例一: (K=图书馆学 OR K=情报学) AND A=范并思 范例二:J=计算机应用与软件 AND (U=C++ OR U=Basic) NOT M=Visual
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.
正在载入数据...
正在载入数据...
正在载入数据...
正在载入数据...
正在载入数据...
正在载入数据...
正在载入数据...
正在链接到云南高校图书馆文献保障联盟下载...
云南高校图书馆联盟文献共享服务平台 版权所有©
您的IP:216.73.216.7