2-取代间苯二酚化合物的合成  

Synthesis of 2-Substituted Resorcinols

作　　者：李彬[1] 张天永[1] 池立峰[1] 夏文娟[1] 

机构地区：[1]天津大学化工学院,天津300072

出　　处：《天津大学学报》2008年第8期1005-1009,共5页Journal of Tianjin University(Science and Technology)

基　　金：教育部留学回国人员科研启动基金(教外司留[2007]247号)

摘　　要：采用改进工艺,以间苯二酚(DHB)和叔丁醇(TBA)为原料合成重要有机中间体2-取代间苯二酚.DHB经过二叔丁基化、异丙基化和脱二叔丁基化3步反应合成了PDHB.在65～70,℃,以酸性阳离子交换树脂(商品名NKC-9)作为催化剂,DHB与TBA反应合成4,6-二叔丁基间苯二酚(BDHB)的收率和纯度分别为85.8%和98.77%.BDHB与溴代异丙烷在NaOH水溶液中,于70,℃反应5～6,h,生成2-异丙基-4,6-二叔丁基间苯二酚(PBDHB),收率和纯度分别为61.6%和96.53%.PBDHB在浓硫酸催化下,以二氯甲苯作为溶剂,经脱叔丁基反应得到PDHB,收率和纯度分别为76.7%和96.14%.改进后工艺可以合成收率、纯度均较高的PDHB,同样可以合成2-乙基(丁基、苄基)间苯二酚.The synthetic technology of an important organic intermediate 2-isopropyl-1,3-dihydroxybenzene （PDHB） with t-butyl alcohol （TBA）and 1,3-dihydroxybenzene （DHB）was improved. PDHB was prepared from DHB by a three-step reaction including di-t-butylation, isopropylation and de-t-butylation. First,4,6-di-t-butyl-1,3- dihydroxybenzene （BDHB） was prepared through alkylation of DHB by TBA at 65-70 ℃ in the presence of acidic ion-exchanged resin （commercial name NKC-9）as the catalysts, and the yield and purity was 85.8% and 98.77%, respectively. Then, BDHB reacted with 2-bromo propane for 5-6 h at 70 ℃ in aqueous alkali to produce 2-isopropyl- 4, 6-di-t-butyl-1,3-dihydroxybenzene （PBDHB）with 61.6% yield and 96.53% purity. Finally ,by means of de-t- butylation,PDHB was catalyzed in the presence of H2SO4 in dichlorotoluene as a solvent. The yield and purity of PDHB was 76.7% and 96.14%,respectively. PDHB of high yield and purity can be prepared by the improved technology, and 2-ethyl （butyl, benzyl ） resorcinols can also be prepared by the similar routes.

关 键 词：4 6-二叔丁基间苯二酚 2-异丙基-4 6-二叔丁基间苯二酚 2-异丙基间苯二酚 酸性离子交换树脂 溴代异丙烷 

分 类 号：TQ243.12[化学工程—有机化工]