实验科学与技术
實驗科學與技術
실험과학여기술
EXPERIMENT SCIENCE AND TECHNOLOGY
2012年
1期
40-42
,共3页
对二甲苯环二聚体%合成%工艺%正交试验法
對二甲苯環二聚體%閤成%工藝%正交試驗法
대이갑분배이취체%합성%공예%정교시험법
[2%2]-paracyclophane%synthesis%process%orthogonal experiment
以对甲基苄基三甲基氯化铵为原料,按Hofmann消除法合成了对二甲苯环二聚体,利用IR、HNMR及熔点测试等对产物结构进行了表征;利用正交试验法对合成工艺进行了优化,得到最佳工艺条件为：季铵盐的浓度220.0 g/L;NaOH的浓度240.0 g/L;反应温度110℃;反应时间10 h,在最佳工艺条件下产物的产率达到35.2,较同类方法提高了10以上。
以對甲基芐基三甲基氯化銨為原料,按Hofmann消除法閤成瞭對二甲苯環二聚體,利用IR、HNMR及鎔點測試等對產物結構進行瞭錶徵;利用正交試驗法對閤成工藝進行瞭優化,得到最佳工藝條件為：季銨鹽的濃度220.0 g/L;NaOH的濃度240.0 g/L;反應溫度110℃;反應時間10 h,在最佳工藝條件下產物的產率達到35.2,較同類方法提高瞭10以上。
이대갑기변기삼갑기록화안위원료,안Hofmann소제법합성료대이갑분배이취체,이용IR、HNMR급용점측시등대산물결구진행료표정;이용정교시험법대합성공예진행료우화,득도최가공예조건위：계안염적농도220.0 g/L;NaOH적농도240.0 g/L;반응온도110℃;반응시간10 h,재최가공예조건하산물적산솔체도35.2,교동류방법제고료10이상。
[2,2]-paracyclophane has been synthesized by the method of Hofmann elimination with quaternary ammonium salt as raw materials.The structure of synthesized product was characterized by IR,HNMR as well as melt peint test.Synthetic process was optimized by orthogonal experiment and best technology parameters were the concentration of quaternary ammonium salt 220.0 g/L,NaOH 240.0 g/L,reaction temperature 110℃ and reaction time 10h.The yield of 35.2 was reached with best technology parameters.The yield obtained by our method is 10 and is much higher than other methods.
