2986-00-7Relevant articles and documents
Chlorination process of prothioconazole intermediate
-
Paragraph 0020-0029, (2021/03/13)
The invention belongs to the field of chemical synthesis, and relates to a chlorination process of a prothioconazole intermediate, in particular to a method for synthesizing the prothioconazole intermediate by using novel equipment, which comprises the following steps of: pumping an organic solvent solution of a raw material alpha-acetyl-gamma-butyrolactone into a micro-channel reactor by using ametering pump by using a micro-channel reactor synthesis device; introducing chlorine into the micro-channel reactor, performing cooling and mixing to obtain an intermediate reaction solution, and performing separating to obtain a prothioconazole intermediate. According to the present invention, the chlorination process has characteristics of easy operation, rapid reaction, less three-waste, low cost, high reaction yield, high content, safety, and easy industrial production.
Synthesis method of beta-chloro-alpha, gamma-dicarbonyl compound
-
Paragraph 0036-0038; 0054-0056; 0060-0062, (2021/03/31)
The invention relates to the technical field of chemical synthesis, and particularly discloses a synthesis method of a beta-chloro-alpha, gamma-dicarbonyl compound. The synthesis method comprises thefollowing steps: under a solvent-free condition, taking an alpha, gamma dicarbonyl compound shown as a formula (I) as a raw material, taking anhydrous aluminum chloride as a catalyst, and introducingchlorine to carry out chlorination reaction, so as to obtain the beta-chlorinated alpha, gamma dicarbonyl compound shown as a formula (II). The beta-chloro-alpha, gamma-dicarbonyl compound shown in the formula (II) is prepared through a chlorination reaction by taking chlorine as a chlorination reagent and taking anhydrous aluminum chloride as a catalyst under a solvent-free condition, a product with the purity of more than 90% can be obtained only through simple post-treatment of a reaction product, the yield can reach 90% or above. The method has the advantages of mild reaction conditions, simple process operation, no generation of sulfur dioxide polluting the environment, greenness, environmental protection, and suitableness for large-scale industrial production.
Preparation method of alpha-chloro-alpha acetyl-gamma-butyrolactone
-
Paragraph 0043; 0058; 0060-0061; 0062; 0064-0065; 0067; 0069, (2021/02/06)
The invention provides a preparation method of alpha-chloro-alpha acetyl-gamma-butyrolactone, wherein the method comprises the following steps: reacting gamma-butyrolactone, an acylation reagent and an alkaline reagent as raw materials, carrying out chlorination reaction, and carrying out after-treatment to obtain alpha-chloro-alpha acetyl-gamma-butyrolactone. According to the preparation method of alpha-chloro-alpha-acetyl-gamma-butyrolactone, introduction of an acid-binding agent in a chlorination reaction is reduced, consumption of phosphoric acid and alkali is avoided, meanwhile, a distillation purification step is omitted, the preparation process is simplified, the amount of waste salt generated in the preparation process is greatly reduced, the preparation cost is effectively reduced, the generation of industrial three wastes is reduced, and a product with relatively high purity and yield is also prepared.