Font Size: a A A

Preparation Of Acid Task Specific Ionic Liquids And Its Application In The Synthesis Of Perfume

Posted on:2011-10-16Degree:MasterType:Thesis
Country:ChinaCandidate:H Y SunFull Text:PDF
GTID:2121360332956360Subject:Applied Chemistry
Abstract/Summary:PDF Full Text Request
This article studied the synthesis of task specific ionic liquids and its application in the synthesis of perfume and achieved some significant results.1. In this article three acid task specific ionic liquids are synthesized . The results are as follows:(1) the proper reaction conditions of intermediate of 1-(4-sulfonic group) butyl-3-methylpyrazine tetrafluoroborate ([4-sulfbmpyrazine][BF4])is the ratio of mol n (2-methylpyrazine)∶n (1,4-butanesultone) = 0.05∶0 .10 ,an amount of solvent acetonitrile of 45 mL, a reaction time of 12 h and heated refluence. The yield could reach 83.5 %.(2) the proper reaction conditions of 1-(4-sulfonic group) butyl-3-methylpyrazine tetrafluoroborate ([4-sulfbmpyrazine][BF4])is a ratio of mol n (intermediate)∶n (HBF4) = 0.05∶0.06 , a reaction temperature of 60℃and a reaction time of 2 h . The yield could reach 92.4%.(3) the proper reaction conditions of intermediate of 1-(4-sulfonic group) butyl-3-methylimidazole tetrafluoroborate([4-sulfbmim][BF4])is a ratio of mol n (2-methylimidazole)∶n (1,4-butanesultone) = 0.10∶0.10 , a reaction time of 6.5 h , heated refluence. The yield could reach 92.8 %.(4) the proper reaction conditions of 1-(4-sulfonic group) butyl-3-methylimidazole tetrafluoroborate([4-sulfbmim][BF4])is a ratio of mol n (intermediate)∶n (HBF4) = 0.10∶0 .10 , a reaction time of 10 h and heated refluence . The yield could reach 85.7%.(5) the proper reaction conditions of 1-(4-sulfonic group) butyl-3-methylimidazole chloride([cmmim] [Cl])is a ratio of mol n (2-methylimidazole)∶n (chloroactic acid) = 0.05∶0 .05 , a reaction time of 8 h , and a reaction temperature of 70℃. The yield could reach 88.9 %.(6) the proper reaction conditions of 1-carboxymethyl-3- methylimidazolium tetrafluoroborate ([cmmim][BF4]) is a ratio of mol n ([cmmim] [Cl])∶n (NaBF4) = 0.05∶0 .05 , a reaction time of 12 h , and a reaction temperature of 80℃. The yield could reach 93.0 %.2. Some ketals and acetals for example cyanophyll, hyacinthol, fructone, ramification of fructone, cyclohexanone ketal and benzaldehyde propylene glycol acetal are synthesized using acid task specific ionic liquids as catalyst. The proper reaction conditions were identified by experiments. The acid task specific ionic liquids ionic liquid had better catalytic activity compared with the traditional acidic catalyst. And it could be recycled and the catalytic activity didn't reduce. The results are as follows:(1) the proper reaction conditions of cyanophyll is a ratio of mol n (benzyl alcohol)∶n (acetal) = 0.10∶0.80 ,an amount of catalyst of 0.4 g, a reaction time of 1 h and a reaction temperature of 20℃. The yield could reach 92.2 %.(2) the proper reaction conditions of hyacinthol is a ratio of mol n (phenethyl alcohol)∶n (acetal) = 0.10∶0.50 ,an amount of catalyst of 0.6 g, a reaction time of 6 h and a reaction temperature of 60℃. The yield could reach 80.3 %.(3) the proper reaction conditions of fructone is a ratio of mol n (ethyl acetoacetate)∶n (ethylene glycol) = 0.10∶0.15 ,an amount of catalyst of 0.5 g, a reaction time of 2 h and an amount of cyclohexane as carrying - water reagent of 40 mL. The yield could reach 95.4%.(4) 5 kinds of ramifications of fructone are synthesized using [4-sulfbmim][BF4] as catalyst. The catalyst had a fairly high catalytic activity and high yield.(5) 4 kinds of ramifications of cyclohexanone ketal are synthesized using [4-sulfbmim][BF4] as catalyst. The catalyst had a fairly high catalytic activity and high yield.(6) the proper reaction conditions of benzaldehyde propylene glycol acetal is a ratio of mol n (benzaldehyde)∶n (1,2-propanediol) = 0.05∶0.08 ,an amount of catalyst of 0.3 g, a reaction time of 6 h , and an amount of cyclohexane as carrying - water reagent of 10 mL. The yield could reach 93.6%.3. 2 kinds of ester (citronellyl propionate, linalyl acetate) are synthesized using acid task specific ionic liquid [4-sulfbmpyrazine][BF4] as catalyst. The proper reaction conditions were identified by experiments. The acid task specific ionic liquids ionic liquid could be recycled and the catalytic activity didn't reduce. The results are as follows:(1) the proper reaction conditions of citronellyl propionate is a ratio of mol n (citronellol)∶n (propionic anhydride) = 0.05∶0.10 ,an amount of catalyst of 0.3 g, a reaction time of 2 h , an a reaction temperature of 70℃. The yield could reach 95.3%.(2) the proper reaction conditions of linalyl acetate is a ratio of mol n (citronellol)∶n (Propionic anhydride) = 0.05∶0.10 ,an amount of catalyst of 0.3 g, a reaction time of 6 h , an a reaction temperature of 30℃. The yield could reach 64.7%.4. Indole derivatives are synthesized using acid task specific ionic liquid [cmmim] [BF4] as catalyst. The proper reaction conditions were identified by experiments. The acid task specific ionic liquids ionic liquid could be recycled and the catalytic activity didn't reduce .
Keywords/Search Tags:acid task specific ionic liquid, acid catalyst, the synthesis of perfume, ketal reaction, acetalization, esterification, Fisher indole synthesis
PDF Full Text Request
Related items