30 results about "Thiophosgene" patented technology

The invention provides a novel Lesinurad midbody and provides a synthesis process of Lesinurad, which is economic, efficient, safe, environment-friendly and applicable to large-scale industrial production. The invention further provides a method for preparing the conventional Lesinurad midbody and Lesinurad by using the novel Lesinurad midbody. When synthesized from the novel Lesinurad midbody provided by the invention, the Lesinurad has advantages that the price of necessary raw materials is low, the raw materials are easy to obtain, heavy metal and solvents which are harmful to the environment are not used, the midbody and a product can be easily separated and purified, the operation is easy, application of thiophosgene which is high in toxicity and not easy to operate is avoided, and the total reaction yield is approximate to or higher than that in the prior art.

The present invention relates to hexa-alkyl guanidine salt ion liquid and its preparation process. The materials 1 ,3-dimethyl-2-imidazolinone and tetra-alkyl urea are produced into intermediate Wilsman salt under the action of phosphorus oxychlooride, oxalyl chloride, thiophosgene, phosgene or dichluoro sulfoxide; the intermediate is then reacted with C10 below aliphatic amine to produce penta-alkyl guanidine; and penta-alkyl guanidine is finally reacted with alkyl bromide or alkyl iodide and methyl or ethyl ester to produce hexa-alkyl guanidine salt ion liquid. The bromine salt and iodine salt may further reacted with various inorganic salt to produce hexa-alkyl guanidine salt ion liquid containing various negative ions. The present invention lays down foundation for the research and development of ionic liquid and provides systemic technology for the industrial production of hexa-alkyl guanidine salt ion liquid..

The invention discloses an isotope labeling reagent which is an isothiocyanopyrimidine isotope labeling reagent with a chemical name of [d0]/[d6]-4,6-dimethoxine-2-isothiocyanate. The preparation method of the reagent comprises the following steps of: firstly, reacting 4,6-dichloro-2-amiopyrimidine with sodium methoxide/deuterosodium methoxide to obtain a [d0]/[d6]-4,6-dimethoxy-2-amiopyrimidine crude product; carrying out reflux reaction on the obtained crude product, thiophosgene and sodium bicarbonate to obtain a final crude product; and then carrying out column chromatography to obtain the isotope labeling reagent disclosed by the invention. The isotope labeling reagent disclosed by the invention can be applied to the identification analysis of polypeptide N-end residues and the quantitative analysis of protein, can speed up the labeling reaction rate and improve a signal of the labeled peptide section, is beneficial to strengthening the accuracy and the credibility of the identified peptide section and has the advantages of less molecular weight of the labelled part, relative simple structure, stable performance, simpleness and convenience for operation, and the like.

The invention discloses a novel method for compounding a medicament of Enzalutamide for resisting the prostate cancer, belongs to the technical field of pharmacy synthetic technique, and particularly relates to novel technique for compounding Enzalutamide. Most of known methods for compounding Enzalutamide relate to use of highly toxic and mephitical thiophosgene and highly toxic oxobutyronitrile and have great difficulty in industrialization. According to the invention, a non-toxic and harmless Lawesson's agent is adopted, and a key parent nucleus of a carbonyl group is subjected to a sulfenylation reaction, so that thiophosgene and oxobutyronitrile are effectively avoided. The reaction condition of the method is mild, and the yield is relatively high, therefore, the novel method has a great industrialization prospect.

A method for producing a trifluoromethyl thioalkyl compound represented by general formula (1) (wherein R represents a C1-C10 alkyl group which may be substituted by R1, or the like; R1 represents a C1-C4 alkyl group or the like; and R2 represents a hydrogen atom, a halogen atom, a C1-C4 alkyl group or the like), which is characterized by adding thiophosgene at an addition temperature of 45 DEG C or more for an addition time of 0.25 hour or more in the presence of a compound represented by general formula (2) (wherein R is as defined in general formula (1); and L represents a halogen atom, a C1-C4 alkylsulfonyloxy group or the like) and a fluorine compound.

The invention relates to the field of compound synthesis, in particular to a method for synthesizing substituted m-phthalic isothiocyanate by a one-pot method, and a synthesized substituted m-phthalic isothiocyanate compound. According to the method, m-phenylenediamine, m-phenylenediamine derivatives and thiophosgene are used as raw materials, triethylamine is used as acid-binding agents, and the one-pot method is used for synthesizing the substituted m-phthalic isothiocyanate. Compared with the prior art, the method provided by the invention utilizes m-phenylenediamine and m-phenylenediamine derivatives and has the advantages that 1) the multi-step reaction is changed into the one-step reaction; 2) the post treatment is simple, and the operation is easy; 3) the reaction condition is mild; 4) the yield is high; 5) the cost is reduced; 6) the micro reaction is changed into the massive reaction, and the method is suitable for industrial production; and 7) the application is wide, and the method is applicable to reaction of various substituted amine.

The present invention discloses a method for synthesizing 4-(4-cyclopropylnaphthalen-1-yl)-1H-1,2,4-triazole-5(4H)-thione. The method includes the following steps: using 4-cyclopropyl-1-naphthylamine (formula A) as a starting reactant, reacting the formula A with carbon disulfide to generate 4-cyclopropyl-1-naphthylamino dithiocarbamate (formula B) under a organic alkaline condition, reacting the formula B with bis (trichloromethyl) carbonate (BTC) or acylating reagents like ethyl chloroformate and methyl chloroformate, etc. to generate 4-cyclopropyl-1-naphthylamino dithiocarbamate chloro-carbonic acid anhydride, conducting decomposition reaction to the resulting product without separation and purification to produce 4-cyclopropyl-1-naphthyl isothiocyanate. The method uses carbon disulfide instead of thiophosgene with greater toxicity, and provides simple process and stable reaction. Furthermore, raw materials are readily available, and industrialization is easy to be realized with a total recovery of more than 65%.

The invention relates to a chelate of isothiocyanate phenyl pentaazacyclo tetraacetic acid and a method for preparing the same. The method comprises the following steps of condensation, hydrolysis, and substitution, the product of which undergoes condensation with bromoacetate, and chelating with a lanthanide to produce p-nitrobenzene pentaazacyclo tetraacetic acid which undergoes deoxidization with 5 percent Pd/C and finally the reaction with thiophosgene to obtain the target compound I. The chelate of isothiocyanate phenyl pentaazacyclo tetraacetic acid is an unknown compound, and the formed rigid aperture compound is chelated with the lanthanide including europium, indium, scythe, and terbium, and the structure of the chelate is determined through element analysis, analysis with infrared and ultraviolet, magnetic resonance imaging, and mass spectrum, the prepared chelate is mainly used for time-resolved fluoroimmunoassay.

The invention belongs to the technical field of medicines, and particularly relates to a synthesis method of 1-(2-dimethylaminoethyl)-5-mercaptotetrazole. The method comprises the following steps: reacting N, N-dimethylethylenediamine with thiophosgene to obtain isothiocyanate, reacting isothiocyanate with azidotrimethylsilane to obtain 1-(2-dimethylaminoethyl)-5-mercaptotetrazole hydrochloride, dissolving 1-(2-dimethylaminoethyl)-5-mercaptotetrazole hydrochloride in water, and carrying out decolorizing and crystallizing to obtain 1-(2-dimethylaminoethyl)-5-mercaptotetrazole. According to themethod, the isothiocyanate is synthesized from the N, N-dimethylethylenediamine and the thiophosgene through a one-step method, so that the synthesis process is simplified and the yield is greatly increased; non-toxic azidotrimethylsilane is used for replacing virulent sodium azide in the cyclization process, so that the safety of the process is improved, and the method is more suitable for industrial amplification.

The invention relates to a chemical synthesis method of 4-methanesulfonylbutyl isothiocyanate (Erysolin). The method comprises that 1-bromo-4-chlorobutane and hydrous sodium methyl mercaptide as starting raw materials undergo a reaction to produce chlorothioether, the chlorothioether and phthalimide potassium salt undergo a reaction to produce a tertiary amine conjugate, the tertiary amine conjugate undergoes a hydrazinolysis reaction to produce thioether primary amine, the thioether primary amine forms isothiocyanate under action of thiophosgene, and the isothiocyanate is oxidized to form Erysolin. The chemical synthesis method is simple in operation, uses a small amount of dangerous reagents, gives consideration to a cost and a yield and is suitable for Erysolin industrial production.

The present disclosure provides a process for the preparation of perfluoroalkyl sulfenyl chloride by reacting a compound of formula [I] with at least one fluoride compound and thiophosgene.