N-甲基-4-（三正丁基锡）咪唑的合成

论文总字数：20971字

摘 要

以4,5-二碘代咪唑为原料，三步合成N-甲基-4-（三正丁基锡）咪唑的实验，采用不同原料和溶剂，通过改变实验方法，对比参照，最终对其合成过程的反应条件进行优化。第一步使用4,5-二碘代咪唑为原料，加入氢氧化钠和DMS，在30℃下完全反应三个小时后，残余的4,5-二碘代咪唑的纯度是5.02%，并且生成的 4,5-碘-1-甲基咪唑的纯度为94.34%。第二步使用4,5-碘-1-甲基咪唑做原料，分别采用不同溶剂对比实验，最终使用THF做溶剂的4,5-碘-1-甲基咪唑剩余0%,4-碘-1-甲基咪唑的纯度为95.9%。产品纯度为96.59%。收率为85.4%。产品含水量为0.12%。第三步从4-碘-1-甲基咪唑制备N-甲基-4-（三正丁基锡）咪唑，加入i-PrMgCl-LiCl （异丙基氯化锂氯化镁）,接着加入Bu₃SnCl，HPLC显示最终产品N-甲基-4-（三正丁基锡）咪唑的含量为90.27%，残余的Bu₃SnCl减少到0.15%，收率为77.5%。

关键词： N-甲基-4-（三正丁基锡）咪唑；N-甲基咪唑；优化设计；合成

Synthesis of N- methyl -4- (tributyl tin) imidazole

Abstract

N-methyl-4-(tributyl tin) imidazole was synthesized from 4,5- diiodide imidazole through three steps. Different raw materials and solvents are used. The reaction conditions of the synthesis process are optimized by changing the experimental methods and comparing references. The first step to use 4, 5-diiodide imidazole as raw material, add sodium hydroxide and DMS and completely reaction under 30 ℃ after three hours, the residue of the purity of 4, 5-diiodide imidazole is 5.02%, and the generated 4,5-iodine-1- methyl imidazole purity of 94.34%. In the second step,4, 5-iodine-1-methyl imidazole was used as raw material, and different solvents were used for comparison experiments. Finally, the remaining 0% of 4, 5-iodine-1-methyl imidazole was used as solvent in THF, and the purity of 4-iodine-1-methyl imidazole was 95.9%. The purity of the product is 96.59%. The yield was 85.4%. The water content of the product is 0.12%. In the third step, N-methyl-4 - (trinbutyl tin) imidazole was prepared from 4-iodine-1-methyl imidazole, and i-PrMgCl-LiCl (isopropyl lithium chloride magnesium chloride) was added, followed by Bu₃SnCl. HPLC showed that the content of the final product N-methyl-4 - (trinbutyl tin) imidazole was 90.27%.The residual Bu₃SnCl was reduced to 0.15% with a yield of 77.5%.

Keywords: N-methyl-4-(trinbutyl tin) imidazole; N-methyl imidazole; Optimization design; synthetic

目 录

摘要........................................................................................................................................................................I

Abstract..................................................................................................................................................................II

第一章 绪论 1

1.1背景 1

1.2 研究意义及应用前景 1

1.3 材料收集 1

第二章 4,5-碘-1-甲基咪唑的合成与反应优化 3

2.1 4,5-二碘代咪唑到4,5-碘-1-甲基咪唑的实验方法 3

2.2 4,5-二碘代咪唑到4,5-碘-1-甲基咪唑的放大生产实验方法 4

第三章 4-碘-1-甲基咪唑的合成与反应优化 7

3.1 4,5-碘-1-甲基咪唑生成4-碘-1-甲基咪唑的实验方法 7

3.1.1 用DCM做溶剂 7

3.2 4,5-碘-1-甲基咪唑生成4-碘-1-甲基咪唑的对比优化实验方法 8

3.2.1 用四氢呋喃做溶剂 8

3.2.2用二甲基四氢呋喃做溶剂 9

3.2.3 对比实验及数据分析 9

3.3 4,5-碘-1-甲基咪唑生成4-碘-1-甲基咪唑的放大生产实验方法 10

第四章 N-甲基-4-（三正丁基锡）咪唑的合成与反应优化 12

4.1 4-碘-1-甲基咪唑到N-甲基-4-（三正丁基锡）咪唑的实验方法 12

4.1.1 用EtMgBr(乙基溴化镁）做原料 12

4.2 4-碘-1-甲基咪唑到N-甲基-4-（三正丁基锡）咪唑的优化实验 14

4.2.1 使用i-PrMgCl-LiCl（异丙基氯化锂氯化镁）做原料 14

1. 结论与展望 16

5.1 结论... .................................................................................................................................................16

5.2 展望.....................................................................................................................................................16

致谢 17

参考文献 18

第一章 绪论

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