本文選題：丁醚脲 + 8-羥基喹啉銅/DMAP/Cu��； 參考：《南京理工大學(xué)》2015年碩士論文

【摘要】：丁醚脲是一種新型硫脲類殺蟲、殺螨劑。在前人工作的基礎(chǔ)上,本文重新設(shè)計(jì)并優(yōu)化丁醚脲的合成工藝。產(chǎn)物結(jié)構(gòu)經(jīng)核磁H譜、C譜、MS、IR表征。以2,6-二異丙基苯胺為原料,用氫溴酸和雙氧水溴化反應(yīng)制得4-溴-2,6-二異丙基苯胺,當(dāng)反應(yīng)條件為n(H2O2):n(2,6-二異丙基苯胺)=1.30：1,反應(yīng)溫度T--15℃,反應(yīng)時(shí)間t=1.5 h,m(二氯乙烷)：m(2,6-二二異丙基苯胺)=12：1時(shí),產(chǎn)品收率為89.6%,純度97.1%。以8-羥基喹啉銅,銅,4-二甲氨基吡啶(DMAP)為復(fù)合催化劑,二甲苯為溶劑,氫氧化鉀為縛酸劑,4-溴-2,6-二異丙基苯胺與苯酚發(fā)生Ullmann偶聯(lián)反應(yīng)制得2,6-二二異丙基-4-苯氧基苯胺,當(dāng)反應(yīng)條件為n(4-溴-2,6-二異丙基苯胺)：n(8-羥基喹啉銅)：n(DMAP):n(Cu)=1：167.5：57.2：74.4,反應(yīng)時(shí)間t=3 h,n(苯酚)：n(4-溴-2,6-二異丙基苯胺)=1.1：1,反應(yīng)溫度T=145℃時(shí),產(chǎn)品收率為80.1%。催化劑可回收套用三次。以水為溶劑,PEG-600為催化劑,2,6-二異丙基-4-苯氧基苯胺與CS2反應(yīng)制備2,6-二異丙基-4-苯氧基苯基氨基二硫代甲酸鹽,當(dāng)反應(yīng)條件為n(2,6-二二異丙基-4-苯氧基苯胺)：n(CS2)：n(三乙胺)=1：3：3,反應(yīng)溫度T=35℃,反應(yīng)時(shí)間t=1.5 h時(shí),產(chǎn)品純度為91.3%,收率87.1%。以二氯甲烷為溶劑,2,6-二異丙基4-苯氧基苯基氨基二硫代甲酸鹽與對甲苯磺酰氯(TsCl)反應(yīng)制得2,6-二二異丙基-4-苯氧基苯基異硫氰酸酯,當(dāng)反應(yīng)條件為n(2,6-二二異丙基-4-苯氧基苯基硫代氨基甲酸鹽)：n(TsCl)=1:1.2,反應(yīng)溫度為T=40℃時(shí),產(chǎn)品純度為86.1%,收率79.7%。以甲苯為溶劑,2,6-二二異丙基-4-苯氧基苯基異硫氰酸酯與叔丁胺發(fā)生親核加成反應(yīng)制備目標(biāo)產(chǎn)物丁醚脲,當(dāng)反應(yīng)條件為n(叔丁胺)：n(異硫氰酸酯)=1.4：1,反應(yīng)時(shí)間t=12 h時(shí),經(jīng)純化后,產(chǎn)品純度為98.6%,收率75.2%。
[Abstract]:Butyl ether urea is a new thiourea insecticide and acaricide. Based on the previous work, the synthesis process of butyl ether urea was redesigned and optimized. The structure of the product was characterized by NMR, H, C and MS IR spectra. 4-bromo-2-diisopropylaniline was prepared by bromination of hydrobromic acid with hydrogen peroxide. The reaction conditions were as follows: NH _ 2O _ 2: n _ 2O _ 2: n _ 2O _ 2-diisopropylaniline was 1.30: 1 and the reaction temperature was T _ (15) 鈩，

本文編號：2003430