對三氟甲基苯腈的合成

制藥工程論文編號:ZY031    論文字數:7844,頁數:19

目  錄
中文摘要 I
英文摘要 II
目錄 III
1. 緒論 1
 1.1 含氟化合物的特征及用途 1
 1.2 含氟農藥中間體 1 
 1.3 對三氟甲基氯苯簡介 2
 1.4 對三氟甲基苯腈 3
2. 實驗部分 5
 2.1 化學試劑和儀器 5
6
 2.2 實驗步驟 6
 2.3 氣相色譜（GC）檢測條件 7
3. 結果與討論 7
 3.1 催化劑的制備條件優化 7
 3.3 對三氟甲基苯腈產品的含量分析及結構鑒定結果 10
4．總結與展望 13
致謝 15
參考文獻 16

摘 要：介紹了含氟化合物的特性，結合當今農業中含氟農藥的應用現狀，闡述研究含氟農藥中間體的意義。對農藥中間體對三氟甲基苯腈的合成進行了探索性研究。以對三氟甲基氯苯與氰化鈉在活性膦鎳[Ni(PPh3)3]催化劑下發生均相催化反應，得到的產物進行精餾分離提純，即得對三氟甲基苯腈。催化劑中鎳鹽、三苯基膦與還原劑鋅粉的最佳配比為1:3:9，催化反應的原料比Ni(PPh3)3: 對三氟甲基氯苯:氰化鈉為1:31:34，以對三氟甲基氯苯計收率達到52.6%。采用紅外光譜、質譜、氣相、氫核磁共振譜等手段對產物結構進行分析鑒定。該結果對開發實際生產技術具有一定的指導作用。
關鍵詞：含氟農藥中間體；對三氟甲基氯苯；對三氟甲基苯腈；均相催化；膦鎳催化劑 
 
Abstract: This article describes the characteristics of fluorine-containing compounds, and explain the significance of fluoride pesticide intermediates, combining with the current application status of fluorine-containing pesticides. Special attention to the pesticide intermediates 4-trifluoromethyl benzonitrile synthesis is drawn. 4-Chlorobenzotrifluoride and sodium cyanide in the activity of nickel-phosphine catalyst [Ni(PPh3)3] have the homogeneous catalysis reactions, The product obtained by distillation separation and purification, that get 4-trifluoromethyl benzonitrile. Nickel salt, triphenylphosphine and zinc have the best molar ratio of 1:3:9, raw material [Ni(PPh3)3], 4-chlorobenzotrifluoride and NaCN feed ratio of 1:31:34 .the yield reached 52.6%. The IR, MS, GC, 1HNMR will be prepared for structural analysis and identification of pure product. .This study optimizes the reaction conditions and improves the conversion rate and selectivity, increased industrial applicability.

Keywords：Fluoride pesticide intermediates; 4-chlorobenzotrifluoride; 4-trifluoromethyl benzonitrile; Homogeneous catalysis, Phosphine nickel catalyst