7 results about "Methyl chloroformate" patented technology

The invention belongs to the field of Velciguat synthesis, and particularly relates to a preparation method of Velciguat and an intermediate product thereof. The preparation method of the Velciguat comprises the following steps: (1) reacting aminomalononitrile with methyl chloroformate to generate an intermediate product I; (2) carrying out ring closing on the intermediate product I and formamidine under an alkaline condition to obtain an intermediate product II; (3) carrying out bromination reaction on the intermediate product II and N-bromosuccinimide to obtain an intermediate product III; (4) reacting the intermediate product III with bis (pinacolato) diboron under the action of a catalyst to obtain an intermediate product IV; and (5) carrying out a reaction on the intermediate product IV and 5-fluoro-1-(2-fluorobenzyl)-3-iodo-1H-pyrazolo [3, 4-b] pyridine to prepare the viriciguat. The method is simple to operate, low in cost and safe in production. The invention also provides the intermediate product obtained by the preparation method.

The invention discloses a purification process of hexazinone production wastewater, and relates to the technical field of wastewater treatment. The process comprises the following steps: introducing wastewater of a hexazinone production process into an enamel microfiltration reactor for reaction, and filtering out pretreated wastewater; the pretreated wastewater is pumped into a graphite condensation type oxidation tower, a composite catalyst composed of a sodium methoxide methanol solution and methyl chloroformate is added for a reaction, and oxygenated wastewater is obtained; adjusting the pH value of the wastewater subjected to oxygen catalysis to 7.0-7.5, introducing the wastewater into a biological denitrification reaction tank, and adding a microbial agent compounded by nitrifying bacteria and denitrifying bacteria for reaction to obtain purified wastewater; refluxing 80% of the purified wastewater to a raw material preparation process for hexazinone production for reuse, and discharging the remaining 20% of the purified wastewater after being detected to be qualified; according to the invention, a grading process of pretreatment, catalytic oxidation, biological denitrification and reclaimed water reuse is designed, so that deep purification of high-ammonia-nitrogen COD wastewater is realized.

The invention relates to a green synthesis method of carbendazim. The method comprises the following steps: (1) taking an o-phenylenediamine solution and a cyanamide solution as raw materials, and carrying out condensation cyclization reaction to generate an intermediate 2-aminobenzimidazole; and (2) mixing the 2-aminobenzimidazole obtained in the step (1) with dimethyl carbonate, and carrying out selective methoxycarbonylation reaction in the presence of a basic catalyst to obtain a reaction product containing carbendazim. According to the method, a biodegradable green reagent dimethyl carbonate is adopted to replace highly toxic methyl chloroformate and upstream phosgene which are required to be used in a traditional process, so that the green, safe and environment-friendly process is guaranteed from the source.

The application belongs to the field of vixepiromide synthesis, and particularly relates to a preparation method of vixepiromide and intermediate products thereof. The preparation method of vixepiromide comprises the following steps: (1) reacting aminopropandinitrile with methyl chloroformate to generate an intermediate product one; (2) ring closing the intermediate product one with formamidine under alkaline conditions to generate an intermediate product two; (3) performing bromination on the intermediate product two with N-bromosuccinimide to generate an intermediate product three; (4) reacting the intermediate product three with pinacol diboron under the action of a catalyst to generate an intermediate product four; and (5) reacting the intermediate product four with 5-fluoro-1-(2-fluorobenzyl)-3-iodo-1H-pyrazolo[3,4-b]pyridine to generate vixepiromide. The application has the advantages of simple operation, low cost and safe production. The application further provides the intermediate products generated in the above preparation method.

This invention relates to a method for the efficient preparation of methyl cyanurate, belonging to the technical field of pharmaceutical intermediate synthesis. The method includes the following steps: mixing 1-hydroxyethyl-3-methylimidazolium acetate with a 28-32% potassium phosphate aqueous solution at a mass ratio of (2.8-3.2):1, followed by allowing the mixture to stand and separate into upper and lower phases; adding a cyanamide aqueous solution to the lower phase; and continuously adding methyl cyanurate to the upper phase; stirring the reaction at 40-50°C for 1.5-2.5 hours; allowing the mixture to stand and separate into upper organic and lower brine phases; diluting the upper organic phase with 1.8-2.2 times its volume of deionized water, precipitating a solid, followed by filtration; collecting the filter cake and filtrate; washing and drying the filter cake to obtain methyl cyanurate. This invention achieves directional distribution of reactants, precise suppression of side reactions, and efficient separation of products by constructing a two-phase aqueous system.

The invention discloses a thiophanate-methyl synthesis method, and relates to the technical field of pesticide synthesis, and the thiophanate-methyl synthesis method comprises the following steps: S1, dissolving sodium thiocyanate in water, adding a catalyst, adding methyl chloroformate, and after the reaction is finished, carrying out liquid separation to obtain methyl isothiocyano formate; s2, methyl isothiocyano formate is added into 1, 2-dichloroethane, and a methyl isothiocyano formate solution is obtained; the preparation method comprises the following steps: adding o-phenylenediamine into 1, 2-dichloroethane, stirring and dissolving, dropwise adding into a methyl isothiocyano formate solution, keeping the temperature to react for 30-60 minutes, cooling and crystallizing, thereby obtaining the o-phenylenediamine methyl isothiocyano formate. The catalyst comprises modified dialkylaniline; the modified dialkylaniline comprises magnesium lithium silicate serving as a carrier, and further comprises dialkylaniline. The thiophanate-methyl synthesized by the method provided by the invention has high yield and content.

The invention discloses a solid-liquid separation process for producing carbendazim, and belongs to the field of pesticide production. The solid-liquid separation process comprises the following process steps: preparing carbendazim through a methyl chloroformate synthesis method to obtain an original feed liquid, performing primary membrane separation, mixing an ethanol water solution, performing secondary membrane separation, recovering and drying to obtain a carbendazim solid. A two-time membrane separation method is adopted for classified screening, primary membrane separation can quickly separate most of carbendazim crystals with conventional sizes in original feed liquid, large-particle-size crystals are prevented from blocking tiny pores of secondary membrane separation, then the carbendazim crystals are blended with an ethanol water solution, the solubility of organic impurities is improved, and the separation efficiency is improved. The method comprises the following steps of: separating crystals by using a membrane, effectively stripping impurities on the surfaces of the crystals, deeply washing the crystals, finally separating by using a secondary membrane, intercepting submicron fine crystals, deeply intercepting the microcrystals in a targeted manner, effectively adsorbing and removing the impurities, and improving the yield and the purity of products.