杀菌剂戊唑醇的合成及表征

Synthesis and Characterization of Fungicide Tebuconazole

以对氯苯甲醛和频哪酮为原料,经缩合、氢化、环氧化和开环反应合成杀菌剂戊唑醇。反应工艺选择了强碱性离子交换树脂为碱性催化剂以及采用CO2中和体系中的碱性物质,使4,4-二甲基-1-(4-对氯苯基)-1-戊烯-3-酮的收率达到98.3%,纯度达到97.4%;开环反应中利用1,2,4-三唑的两种异构体热力学稳定性差异,在强碱性离子交换树脂作用下使用了催化剂N,N-二甲基-4-氨基吡啶,使戊唑醇的纯度达到98.2%,收率达到67%以上。

Using 4-chlorophenyl aldehyde and 3,3-dimethy1-2-butanone as starting material, fungicide tebuconazole was synthesized via condensation, hydrogenation, epoxidation and ring-opening reaction. The yield of 1-（4-chloro-phenyl）-4,4-dimethyl-pent-1-en-3-one can reach 98.3% with the purity of 97.4% （GC） by using strongly basic ion exchange resin as basic catalyst and CO2 as basic material to neutralize the ionized -OH ion. Based on the different thermodynamic stabilities of two isomers of 1,2,4-triazole and under the help of strongly basic ion exchange resin, the tebuconazole yield of 67% with the purity of 98.2% （HPLC） can be reached by using the high selectivity catalyst N,N-dimethyl-4-aminopyridine. Since it has the advantages of having high quality product, stable process technology and less waste gas, water and industrial residue, the proposed synthesis route of tebuconazole has good prospects.