CAJ | 학술논문

取代二苯醚(SDE)化合物是重要的精细化工中间体,它们可由Williamson反应合成.采用室温等离子液体(RIL)作为溶剂,可使Williamson反应的工艺清洁化.合成了一种RIL-1-丁基-3-甲基咪唑六氟磷酸盐(BMIMPF_6),并以它为溶剂、K_2CO_3为催化剂,以取代硝基苯和苯酚为原料,通过Williamson反应合成了一系列SDE.研究了影响醚化反应的一些因素,如温度、时间、催化剂等,并在此研究基础上得出了较佳的醚反应条件为: 物料/催化剂的摩尔比为1/1,温度为100 ℃,时间为1 h.在此条件下所得SDE的收率为70%～93%,产品结构由~1H NMR、~(13)C NMR及MS所证实.另外,RIL至少可循环使用5次,而对SDE的收率及质量无明显影响,有利环保.
취대이분미(SDE)화합물시중요적정세화공중간체,타문가유Williamson반응합성.채용실온등리자액체(RIL)작위용제,가사Williamson반응적공예청길화.합성료일충RIL-1-정기-3-갑기미서륙불린산염(BMIMPF_6),병이타위용제、K_2CO_3위최화제,이취대초기분화분분위원료,통과Williamson반응합성료일계렬SDE.연구료영향미화반응적일사인소,여온도、시간、최화제등,병재차연구기출상득출료교가적미반응조건위: 물료/최화제적마이비위1/1,온도위100 ℃,시간위1 h.재차조건하소득SDE적수솔위70%～93%,산품결구유~1H NMR、~(13)C NMR급MS소증실.령외,RIL지소가순배사용5차,이대SDE적수솔급질량무명현영향,유리배보.
Substituted diphenyl ethers (SDE) belong to an important fine chemical intermediates which can be synthesized via Williamson reactions. Room-temperature ionic liquid (RIL) as solvent could realize clean procedure of SDE′s synthesis. The authors prepared a RIL of 1-butyl-3-methyl imidazolium hexafluorophosphate (BMIMPF_6),and synthesized a series of SDEs from substituted nitrobenze and phenol via Williamson reaction by use of BMIMPF_6 as green solvent and K2CO3 as catalyst. Some factors affecting the etherification,such as temperature,time and catalysts etc,were studied,and the relatively optimal reaction conditions were worked out: molar ratio of reaction material/catalyst=1/1(molar),T=100 ℃,t=1 h. Under the above procedures the yield of resulting SDEs could be 70%-93%,and the structural confirmation was done by ~1H NMR,~(13)C NMR and MS. One additional point should be emphasized that the RIL could be reused at least 5 times without noticeably deteriorating SDE′s yield and purity. This is beneficial to environmental protection.