2,6-二异丙基-4-苯氧基苯基异硫氰酸酯的合成

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

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.