48 results about "Chlorethoxyfos" patented technology

The invention relates to the technical field of drug synthesis, and provides a method for synthesizing 2-fluoro-5-trifluoromethylpyrimidine. The invention uses 5-methyluracil as a raw material, and obtains the target product through a cyclic chlorination reaction, a reduction reaction, a chlorination reaction and a fluorination reaction, the process is simple, the raw materials are cheap and easy to obtain, the yield is high, and no generation of Heavy metal pollution; and the present invention uses phosphorus oxychloride to perform chlorination in the cyclic chlorination reaction, and uses chlorine to perform chlorination in the chlorination reaction, and the costs of both are relatively low, and phosphorus pentachloride is used in the cyclic chlorination reaction. Recovering phosphorus oxychloride can further reduce the reaction cost.

The invention belongs to the technical field of medicine chemosynthesis, and relates to a preparation method of 6-chloro-3-methyluracil. The method comprises the following steps that 1, methylurea, anorganic solvent and alkali are added into a reaction container for stirring and dissolution, then malonic acid or malonic ester is added, heating and reflux are conducted, then cooling is conducted,acid is added to adjust a pH value of reaction liquid, water is added, the reaction liquid is cooled, suction filtration is conducted, and drying is conducted to obtain a white to off-white first intermittent in a shape of loose powder; 2, phosphorus oxychloride is used for chloridizing the first intermittent to obtain a crude product; 3, the crude product prepared in the step 2 is subjected to decoloration by means of activated carbon to obtain a finished product. According to the preparation method of the 6-chloro-3-methyluracil, the product in the step 1 precipitates in a form of sodium salt, that is to say, the first intermittent is 1-sodium methylbarbiturate, compared with the prior art where a first intermittent precipitates in a form of 1-methylbarbituric acid, the preparation method of the 6-chloro-3-methyluracil has the advantages that the yield is obviously improved, moreover, in the step 2, acetonitrile is used as the solvent, the phosphorus oxychloride usage is reduced, post-treatment is convenient, and meanwhile, the product has a good crystal form, and is easy to filter.

The invention discloses a purification method for salifying 1-(4-methoxybenzyl)-3, 4, 5, 6, 7, 8-hexahydroisoquinoline. The method comprises the following steps: allowing N-(2-cyclohexenyl ethyl)-2-(4-methoxyphenyl) acetamide to react with phosphorus oxychloride in xylene to obtain 1-(4-methoxybenzyl)-3, 4, 5, 6, 7, 8-hexahydroisoquinoline, carrying out reduced pressure evaporation to remove xylene and excessive phosphorus oxychloride, and adding a solvent with destroyed phosphorus oxychloride to destroy residual phosphorus oxychloride; and extracting the 1-(4-methoxybenzyl)-3, 4, 5, 6, 7, 8-hexahydroisoquinoline hydrochloride by using halogenated hydrocarbon, carrying out vacuum concentration to remove the solvent, adding a crystallization solvent, and crystallizing to obtain the high-purity 1-(4-methoxybenzyl)-3, 4, 5, 6, 7, 8-hexahydroisoquinoline hydrochloride. The method is convenient and safe in process and high in yield, the content of the arylation compound impurity 1-(4-methoxybenzyl)-5, 6, 7, 8-tetrahydroisoquinoline is low, the amount of three wastes is small, and the method is suitable for industrial production.

The invention relates to an synthesizing method of 2-methyl-7-( substituted pyrimidine-4-amino)-4-(substituted piperazine-1-base) piperidine-1-base) isoindoline-1-ketone and an intermediate thereof, mainly solving the technical problems of overlength single-line synthetic route, difficult separation and purification, low productivity, high synthesizing cost, narrow applicability, and the like of the traditional synthesizing method. The process method comprises the following steps of: carrying out substitution reaction on 2,4,5-trichloropyrimidine as a raw material and sodium methyl mercaptideto generate the intermediate, i.e. 2,5-dichloro-4-methylthiopyrimidine; then carrying out the substitution reaction with aromatic amine to generate the intermediate, i.e. 2-aromatic amino-4-methylthio-5-chloropyrimidine; then hydrolyzing the methylthio to generate the intermediate, i.e. 2-aromatic amino-4-hydroxy-5-chloropyrimidine; enabling a hydroxyl compound to generate dichloride under the action of phosphorus oxychloride; and finally carrying out the substitution reaction with amine to obtain the 2-methyl-7-(5-chlorine-2-aromatic amido-pyrimidine-4-amino)-4-(4-(4-methyl piperazine-1-base) piperidine-1-base) isoindoline-1-ketone under the action of hydrogen chloride ethyl acetate.