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混合溶劑中的高選擇性氯代反應研究

時間:2019-05-05 21:17來源:畢業論文
在苯乙酮的對位添加鹵素、甲基、硝基等7種不同的苯乙酮類底物進行實驗。在普適性實驗中一氯代物產物在78%~95%,其中產率相對較高的是是苯乙酮、對甲基苯乙酮、乙酰乙酸乙酯

摘要:傳統溶劑大多是有害溶劑,但還是有部分溶劑是綠色溶劑例如:乙酸乙酯等,即使是現在也經常應用于綠色化學工藝,但如果使用混合溶劑可以提高單一溶劑所沒有的性能。現有的氯代試劑是氯氣、N-氯代丁二酰亞胺和三氯異氰尿酸等。以氯氣為氯代試劑,氯氣毒性大、操作不便,與綠色化學的要求有一定的距離;以N-氯代丁二酰亞胺(NCS)為氯代試劑,反應選擇性高,產率高,但NCS價格偏高、含氯量較低。以三氯異氰尿酸(TCCA)作為氯代試劑,具有廉價易得、 含氯量高、毒性較低、易于操作的特點。因此本論文用混合溶劑和TCCA進行相關氯代物的合成。
針對國內現有傳統苯乙酮氯化工藝的產率低、操作不便、成本高以及毒性大等一系列缺點,本論文以苯乙酮為底物、三氯異氰尿酸為氯化劑,在有混合溶劑的條件下進行反應。通過調整混合溶劑的種類、TCCA的用量和反應時間的調節,優化該反應的影響因素,以便夠獲得該實驗的最佳條件,得到高產率一氯代苯乙酮的最佳反應條件。通過實驗得到當苯乙酮(1.2 g /10 mmol)、TCCA(0.77 g / 3.33 mmol)和混合溶劑(為乙腈、乙醇和無水硫酸鎂)反應45min時,實際產量最大,得到1.45 g無色油狀物,產率為94.2%。對于羰基同系物廣泛應用的現在,我們對在苯乙酮的對位添加鹵素、甲基、硝基等7種不同的苯乙酮類底物進行實驗。在普適性實驗中一氯代物產物在78%~95%,其中產率相對較高的是是苯乙酮、對甲基苯乙酮、乙酰乙酸乙酯。35193
畢業論文關鍵詞:綠色化學;混合溶劑;一氯代苯乙酮;三氯異氰尿酸;高選擇性;普適性研究
源¥自%六:維;論-文'網=www.aftnzs.live

 Research on selective chlorinated reaction in mixed solvent
Abstract:Most of conventional solvents are poisonous,there are also some parts of them are green solvents like acetic ethe which is often used in green chemical process even in these days.However, the use of component solvents can improve the performance what the single solvents don't have.The chlorinated reagents now  we have are chlorine、N-Chlorosuccinimide and trichloroisocyanuric acid(TCCA) and so on.If we use chlorine as chlorinated reagents,there was a certain distance between the requirements of green chemistry which was because of the toxic and complicate of chlorine.NCS is good chlorinated reagents for its high selectivity and high yield,but the price is higher and with low chlorine content.TCCA has advantages as chlorinated reagents,such as the characteristics of cheap, high chlorine content, low toxicity and easy operation .For these reason ,in this paper we choose component solvents and TCCA to carry on synthesis of relevant chlorine generation.
In view of a series of shortcomings of the domestic existing traditional acetophenone chlorination process of low yield,inconvenient operation, high cost ,toxicity and so on ,this paper will use acetophenone as substrate, cross-linked with different cyanuric acid as chlorinating agent in under the conditions of mixed solvent to get react .By adjusting the types of mixed solvent, adjusting the regulation of TCCA dosage and reaction time,optimizing the influence factors of the reaction,we can easy to get the best condition of the experiment, and get the best reaction conditions of  high yield of chlorinated acetophenone.Through the experiment we can get that when acetophenone (1.2 g / 10 tendency), TCCA tendency for 0.77 g and mixed solvent (for acetonitrile, alcohol and anhydrous magnesium sulfate) get reaction for 45 minutes, the Actual output will be the biggest,and we can get 1.45 grammes of colorless oily matter, the yield was 94.2%.For acetophenone homologue was widely used now, we do the experiment  by adding  seven different phenyl ethyl ketone substrate such as halogen, methyl, nitro in Acetophenone counterpoint.In general experiment ,the one chlorinated yeilds were between 78% and 95%,among them whose Production rate was relatively high was phenyl ethyl ketone, methyl phenyl ethyl ketone, ethyl acetoacetate. 混合溶劑中的高選擇性氯代反應研究:http://www.aftnzs.live/huaxue/20190505/33038.html
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