Study On The Synthesis Of The Key Intermediate Of Prothioconazole

Low toxicity, high level of efficacy, extremely broad-spectrum of activity are the significant features to triazolinthiones fungicide, prothioconazole is the bane of cereal crops with a variety of pests and diseases. In recent years, prothioconazole market has expanded, so the study of prothioconazole of the synthesis process is more and more important. For now, prothioconazole of entire synthesis process research is not very mature.High cost of inputs. Therefore, the synthetic route of prothioconazole was studied to improve the yield of each step of the route to reduce the cost of investment, and its significance is very important. For this reason, through a lot of research and reading literature to optimize the synthesis route prothioconazole key intermediates, specific research works have carried out as follows:1.α- chlorine-γ- acetyl-butyrolactone was successfully synthesized with α- acetyl-γ- butyrolactone and chlorine as raw materials,Under the optimum conditions for synthesis of α- chlorine- γ-acetyl-butyrolactone. LC、GC- MS confirmed α- chloro-α- acetyl--γ-butyrolactone. Under the best conditions.The purity of product was 97.5%, with the yield was 95.7%. In this process, the synthesis of the route is less demanding, and the operation is relatively simple with mild reaction conditions, the yield is relatively high.2. 3, 5- dichloro- 2- pentanone was synthesized with α- chlorine-γ- acetyl-butyrolactone and hydrochloric acid as raw materials under hydrolysis, the open-loop, decarboxylation, chlorination,At the same time,the nitrogen is also important, GC 、 GC-MS confirmed the product,Under the optimal reaction conditions the purity of product was 93.5%, with the yield was 87.6%. Study of the route improved the yield of the product, cost savings, and easier to industrialization.3.1-chloro-1-acetyl-cyclopropane was synthesized with 3,5-dichloro-2-pentanone and sodium hydroxide as raw materials, concentrated tetrabutyl ammonium hydrogen sulfate as a catalyst, Optimization of the synthesis route has improved. GC、GC-MS confirmed 1-chloro-1-acetyl-cyclopropane, under the optimum conditions the purity of this product was 91.8%, with the yield was 86.2%.4.1-chloro-1-chloroacetyl-cyclopropane was synthesized with 1-chloro-l-acetyl-cyclopropane and chloride as the raw materials. After neutralization treatment, the purity of the product was 87.8%, with the yield was 76.6%,GC、1HNMR confirmed 1-chloro-1-chloroacetyl-cyclopropane...