广州化工
廣州化工
엄주화공
GUANGZHOU CHEMICAL INDUSTRY AND TECHNOLOGY
2011年
17期
59-60,85
,共3页
三苯胺%微波辐射%合成
三苯胺%微波輻射%閤成
삼분알%미파복사%합성
triphenylamine%microwave irradiation%synthesis
以氢氧化钾(4)为缚酸剂,CuCl、1,10-菲啰啉(3)为催化剂,在微波辐射条件下,对碘甲苯(1)和对溴苯胺(2)在甲苯(5)中反应合成了4-溴-4',4″-二甲基三苯胺,其结构经1HNMR和IR表征。由正交实验确定最佳工艺条件为:1用量为24 mmol,n(1)∶n(2)∶n(3)=2.4∶1.0∶4.0,微波功率为250 W,于105℃反应120 min,收率77.1%。
以氫氧化鉀(4)為縳痠劑,CuCl、1,10-菲啰啉(3)為催化劑,在微波輻射條件下,對碘甲苯(1)和對溴苯胺(2)在甲苯(5)中反應閤成瞭4-溴-4',4″-二甲基三苯胺,其結構經1HNMR和IR錶徵。由正交實驗確定最佳工藝條件為:1用量為24 mmol,n(1)∶n(2)∶n(3)=2.4∶1.0∶4.0,微波功率為250 W,于105℃反應120 min,收率77.1%。
이경양화갑(4)위박산제,CuCl、1,10-비라람(3)위최화제,재미파복사조건하,대전갑분(1)화대추분알(2)재갑분(5)중반응합성료4-추-4',4″-이갑기삼분알,기결구경1HNMR화IR표정。유정교실험학정최가공예조건위:1용량위24 mmol,n(1)∶n(2)∶n(3)=2.4∶1.0∶4.0,미파공솔위250 W,우105℃반응120 min,수솔77.1%。
4-Bromo-4′,4″-dimethyltriphenylamine was synthesized from 4-Iodotoluene(1) and 4-Bromoanilines(2) in methylbenzene(5) using KOH(4) as an alkali under microwave irradiation.The structure was confirmed by 1HNMR and IR.The optimal reacion conditions by orthogonal experiment were that 1 was 24 mmol,n(1):n(2):n(3) was 2.4:1.0:4.0,microwave power was 250 W at 105 ℃ for 120 min.The yield was 77.1% under the conditions.