2986-00-7Relevant academic research and scientific papers
Preparation method of alpha-chloro-alpha acetyl-gamma-butyrolactone
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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.
Chlorination process of prothioconazole intermediate
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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.
Differences in the efficiency of 3-deazathiamine and oxythiamine pyrophosphates as inhibitors of pyruvate dehydrogenase complex and growth of HeLa cells in?vitro
Grabowska, Ewa,Czerniecka, Magdalena,Czy?ewska, Urszula,Zambrzycka, Aneta,?otowski, Zenon,Tylicki, Adam
, p. 122 - 129 (2020/11/16)
Oxythiamine (OT) and 3-deazathiamine (DAT) are the antimetabolites of thiamine. The aim of study was to compare the effects of OT and DAT pyrophosphates (-PP) on the kinetics of mammalian pyruvate dehydrogenase complex (PDHC) and the in?vitro culture of HeLa cells. The kinetic study showed that 3-deazathiamine pyrophosphate (DATPP) was a much stronger competitive inhibitor (Ki = 0.0026 μM) of PDHC than OTPP (Ki = 0.025 μM). Both Ki values were much lower versus K m for thiamine pyrophosphate (0.06 μM). However, DATPP added to the culture medium for the HeLa cells culture did not hamper the rate of cell growth and showed not significant impact on the viability of the cells, whereas OTPP and OT showed a significant cytostatic effect. The differences between the thiamine antivitamins in their effect on cell growth in?vitro may be due to differences in physicochemical properties and difficulty in DAT transport across the cell membrane.
Synthesis method of beta-chloro-alpha, gamma-dicarbonyl compound
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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.
Fully continuous flow preparation method of 3-chloro-4-amyl oxoacetate
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Paragraph 0005; 0037-0052, (2021/06/22)
The invention belongs to the technical field of organic chemical engineering, and particularly relates to a fully continuous flow preparation method of 3-chloro-4-amyl oxoacetate. The method comprises the following steps of simultaneously conveying chlorine and a reaction solution of acetyl butyrolactone into a micro-channel reactor, and carrying out continuous chlorination reaction to obtain alpha-acetyl-alpha-chloro-gamma-butyrolactone, then continuously conveying the reaction liquid and a mixed solution of glacial acetic acid, hydrochloric acid and water to a micro-reaction system consisting of a next micro-mixer and a micro-channel reactor at the same time, and carrying out continuous acylation reaction to obtain 3-chloro-4-amyl oxoacetate finally, acquiring a final product in a micro-channel system of continuous quenching and continuous extraction separation. Compared with a traditional intermittent kettle type synthesis method, the method disclosed by the invention is short in reaction time, high in product yield, high in automation degree, high in process continuous efficiency, high in space-time yield, low in energy consumption and easy to industrially amplify and apply.
Method for preparing alpha-chloro-alpha-acetyl-gamma-butyrolactone
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Paragraph 0040-0055, (2020/05/01)
The invention relates to the field of organic synthesis, and particularly discloses a method for preparing alpha-chloro-alpha-acetyl-gamma-butyrolactone. The preparation method comprises the followingsteps: (1) in the presence of a solvent, carrying out a salt forming reaction on alpha-acetyl-gamma-butyrolactone and at least one inorganic alkaline substance selected from NaOH, KOH, K2CO3 and Na2CO3 until a precipitate is generated, and then dissolving the precipitate to obtain a first solution; (2) carrying out a contact reaction on the first solution and chlorine to obtain a second solution;and (3) layering the second solution so as to obtain the alpha-chloro-alpha-acetyl-gamma-butyrolactone. The method has the advantages of simple operation, environmental protection, mild reaction conditions, and important practical significance.
Synthetic method of midbody 3,5-dichloro-2-pentanone
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Paragraph 0007; 0017; 0018; 0027, (2018/11/03)
The invention discloses a synthetic method of midoby 3,5-dichloro-2-pentanone. The synthetic method adopts alpha-acetyl-gamma-butyrolactone, anhydrous potassium carbonate, alpha-acetyl-alpha-chloro-gamma-butyrolactone, hydrochloric acid, glacial acetic acid, Cu2O, benzidine and anhydrous THF as main raw materials, adopts alpha-acetyl-gamma-butyrolactone to be converted to the corresponding enol structure under the catalytic effect of the lewis acid-sulfonyl chloride, the chloride ions attach the alpha site of carbonyl, then protons are transferred, hydrogen protons are removed from a hydrogengroup, and then the hydrogen protons are re-arranged and converted to the carbonyl with more stable structure. When the acetic acid is used as a solvent and has certain solubility for an organic phaseand the hydrochloric acid, the reaction is easier, the reaction yield is greatly increased under the effect of a catalyst, the production process of prothioconazole is shortened, and the energy consumption is reduced.
A α - chloro - α - acetyl - γ - butyrolactone preparation method (by machine translation)
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Paragraph 0021; 0022; 0023; 0024; 0025; 0026, (2017/06/02)
The invention discloses a α - chloro - α - acetyl - γ - butyrolactone preparation method. First of all the α - acetyl - γ - butyrolactone is dropped to the low-temperature, then at this temperature into the chlorine, maintain chlorine gas saturated state reaction 5h above, after the reaction stop through chlorine, nitrogen in the system in order to catches up with excess chlorine and hydrogen chloride gas generated by the reaction, and then the aqueous solution of sodium bicarbonate cleaning, to obtain the target product. The present invention under low temperature conditions α - acetyl - γ - butyrolactone react with chlorine to produce the target product, an inexpensive chlorine replaces the chloride and the like traditional chlorinated reagent, avoids the generation of waste gas such as sulfur dioxide, reduces the reaction time, the reaction of the simplified post-processing, the product α - chloro - α - acetyl - γ - butyrolactone yield from 90% increased to 98% or more, greatly reduces the production cost, to c bacterium sulfureum zuo the industrialization of played a positive role in development. (by machine translation)
A 3, 5 - dichloro - 2 - pentanone synthetic method (by machine translation)
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Paragraph 0014; 0015; 0017; 0018, (2017/08/28)
The invention discloses a 3, 5 - dichloro - 2 - pentanone synthesis method, the α - acetyl - γ - butyrolactone to sulfonyl chlorine chloro- by heat after the open loop in the hydrochloric acid solution, decarboxylation, chloro, to obtain the crude product, is distilled under reduced pressure to obtain the high pure 3, 5 - dichloro - 2 - pentanone. The method used at the same time phase transfer catalyst and a Lewis acid catalyst, to avoid black caused by tar, the reaction speed is accelerated, improves the yield of primary alcohol chloro, this line is simple in operation, easy processing, high yield, is suitable for industrial production. (by machine translation)
A 3, 5 - dichloro - 2 - pentanone synthesis process (by machine translation)
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Paragraph 0032; 0033; 0035; 0037; 0039; 0041; 0043; 0045, (2018/04/02)
The invention discloses a 3, 5 - dichloro - 2 - pentanone synthesis process, the process uses water as solvent, α - acetyl - γ - butyrolactone in the double-layer glass reactor in the judgement of the sulfonyl chlorine chloro-, ring opening hydrolysis, decarboxylation, re-chloro continuous reaction, high purity is obtained 3, 5 - dichloro - 2 - pentanone. The method adopts the stage temperature control reaction, compared with the traditional technology does not need to add any catalyst, can make the reaction totally, safety and environmental protection, low cost, high yield reaction at the same time, industrialized the operability is strong, and has good application prospect. (by machine translation)
