22591-21-5Relevant articles and documents
Method for preparing alpha,alpha-dichloroketone under solvent-free condition
-
Page/Page column 7-8, (2021/06/21)
The invention provides a method for synthesizing an alpha,alpha-dichloroketone compound by taking methyl ketone and sulfonyl chloride as raw materials. The method comprises the following steps: heating a reaction mixture of methyl ketone and sulfonyl chloride to 80 DEG C under a dry air condition, stirring for 4-8 hours, after the reaction is finished, removing sulfonyl chloride from the obtained mixture, and carrying out silica gel column chromatography separation by taking ethyl acetate-hexane as an eluent to obtain the alpha,alpha-dichloroketone compound. The synthesis method provided by the invention has the advantages of extremely high chemical reactivity and selectivity, simple and easily available raw materials, low price, simple operation, no need of any catalyst and solvent, reduction of the synthesis cost and the pollution of organic solvents to the environment, greenness, economy and the like.
Novel synthesis method of metribuzin intermediate
-
Paragraph 0015; 0019; 0023, (2020/01/25)
The invention discloses a novel synthesis method of a metribuzin intermediate, wherein the intermediate triazinone of metribuzin is produced by using pinacolone (methyl tert-butyl ketone) as an initial raw material through reaction steps of chlorination, hydrolysis, oxidation, condensation and the like. According to the invention, the reaction conditions are mild, and the total yield reaches 92.4%; hydrogen peroxide is used as an oxidizing agent for replacing sodium hypochlorite, and the oxidation reaction is carried out at a room temperature, so that the operation is convenient, and the byproduct is water so as to avoid the discharge of pollutants such as salt-containing wastewater and the like in the production process; and after the reaction is finished, the intermediate and the catalyst are subjected to chromatographic separation so as to recycle the water phase containing the catalyst.
H2O2/HCl system: Oxidation-chlorination of secondary alcohols to α,α′-dichloro ketones
Nikishin, Gennady I.,Kapustina, Nadezhda I.,Sokova, Lyubov' L.,Bityukov, Oleg V.,Terent'ev, Alexander O.
supporting information, (2020/07/13)
The one-pot oxidation-chlorination of secondary alcohols to give α,α′-dichloro ketones in 62–80percent yields is reported. The convenient and readily available H2O2/HCl system acts on secondary alcohols (C5-C17) with the formation of α,α′-dichloro ketones. The reaction proceeds with high selectivity under the reported conditions; during this process peroxide formation and the Baeyer-Villiger oxidation reactions are not observed.