2，2-二溴-4，4，4-三氟乙酰乙酸乙酯的合成

以四氯化碳为溶剂,三氟乙酰乙酸乙酯和溴素为原料合成了2,2-二溴-4,4,4-三氟乙酰乙酸乙酯,研究了原料配比、反应温度、反应时间等因素对反应的影响,优化了最佳合成工艺条件：171（三氟乙酰乙酸乙酯）：n（溴素）=1：2．6,反应温度为25℃,反应时间20h,产物收率73．9％。产物结构通过。HNMrt和与IR进行了确证。     

Synthesis of N‐Heteroaryl(trifluoromethyl)hydroxyalkanoic Acid Esters by Highly Efficient Solid Acid‐Catalyzed Hydroxyalkylation of Indoles and Pyrroles with Activated Trifluoromethyl Ketones

The synthesis of N‐heteroaryl(trifluoromethyl)hydroxyalkanoic acid esters by solid acid‐catalyzed Friedel–Crafts hydroxyalkylation of indoles and pyrroles with ethyl 3,3,3‐trifluoropyruvate and ethyl 4,4,4‐trifluoroacetoacetate is described. The inexpensive and readily available K‐10 montmorillonite is found to be an efficient catalyst for the synthesis of a wide variety of trifluoromethylated indol‐3‐yl‐ and pyrrol‐2‐yl‐hydroxypropionic and ‐butanoic acid esters. Using a series of substituted indoles and pyrroles the corresponding products were isolated in excellent yield (up to 98%) and 100% selectivity under mild experimental conditions, during very short reaction times. Beyond these, the ease of product isolation, catalyst stability and handling make this process an attractive, environmentally benign alternative for the synthesis of the target compounds.     

4-三氟甲基烟酸的合成工艺

以三氟乙酰乙酸乙酯和氰基乙酰胺为原料,经环合、氯化、氰基水解、催化氢解4步反应得到4-三氟甲基烟酸,总收率达48.3%。其结构经1HNMR、MS分析测试技术确证。通过考察各步反应条件,得出最佳工艺条件为:氯化反应中,n(2,6-二羟基-4-三氟甲基烟腈)∶n(三乙胺)∶n(四甲基氯化铵)=1∶2∶1,产率80.8%;氰基水解的最佳溶剂为体积比4∶1的硫酸-硝酸混合溶剂,产率92.7%;催化氢解反应中,n(2,6-二氯-4-三氟甲基烟酸)∶n(醋酸钠)=1∶2,10%Pd/C的用量为2,6-二氯-4-三氟甲基烟酸质量的6%,产率90.4%。     

吡噻菌胺关键中间体的制备研究进展

总结了文献报道的吡噻菌胺关键中间体1-甲基-3-三氟甲基-1H-吡唑-4-甲酸的制备工艺路线和合成方法。1-甲基-3-三氟甲基-1H-吡唑-4-甲酸主要由三氟乙酰乙酸乙酯进一步反应得到,主要有6条合成路线,其中三氟乙酰乙酸乙酯路线工艺简单、反应条件温和、原料易得等特点,适合工业化生产。