32results about How to "The reaction is easy to scale up" patented technology

The invention relates to a preparation method for bicyclo [1.1.1] pentane-1,3-dicarboxylic acid dimethylester, and mainly solves the technical problem that a method suitable for industrial synthesis does not exist at present. The preparation method comprises the following six steps: firstly, reacting a compound (1) and bromoform under an alkaline condition to obtain a compound (2); secondly, reacting the compound (2) and lithium methide to obtain a compound (3); thirdly, illuminating the compound (3) and diacetyl by a high-pressure mercury lamp to obtain a compound (4); fourthly, treating with sodium hypochlorite to obtain a compound (5); fifthly, reacting the compound (5) and thionyl chloride to obtain a compound (6); and finally, treating the compound (6) under the effect of methanol to obtain a compound (7) which is a final product. A reaction formula is as shown in the specification, and the acquired bicyclo [1.1.1] pentane-1,3-dicarboxylic acid dimethylester is a useful midbody or product for synthesis of many drugs.

The present incention relates to a synthesis method for 4-(tert-butoxycarbonyl) octahydrofuro[3,2-b] pyridine-6-carboxylic acid, and mainly solves the technical problem of no synthesis method suitable for industrialization at present. The synthesis method comprises six steps: first esterifying a compound 1 to obtain a compound 2; then performing iodination to produce a compound 3; acetylating the compound 3 to obtain a compound 4; then performing coupling to obtain a compound 5; performing cyclization to obtain a compound 6; performing hydrogenation to obtain a compound 7, then reacting with Boc anhydride to obtain a compound 8; and performing hydrogenation to obtain a final compound 9. The reaction formula is shown in the description.

The invention relates to a synthesis method of tert-butyl-8-oxo-2,6,9-triazaspiro[4.5]decane-2-formylate. The technical problem that an appropriate industrial synthesis method is inexistent at presentis mainly solved. The synthesis method is divided into two steps: the first step, adding triethylamine in a methanol solution dissolved with a compound 1 and amino ethyl acetate hydrochloride, and then dropwise adding tetraisopropyl titanate in the reaction solution, after completing the dropwise adding, reacting the mixed system for 12 h at 25 DEG C; adding trimethylsilyl cyanide in the reactionsystem at 25 DEG C, and then reacting for 12 h at 25 DEG C, performing post-treatment to obtain a compound 2; and the second step, adding the compound 2, nickel and ammonia water in the methanol solution, and performing hydrogenation to obtain the final compound.

The present invention relates to a 4-tert-butoxycarbonyl-hexahydro-2H-furo [3,2-b] pyrrole-6-carboxylic acid synthetic method and mainly solves a technical problem that currently no suitable industrial synthetic method exists. The synthetic method comprises the following four steps: firstly, a compound 1 is subjected to an alkylation reaction with bromo chloroethane to obtain a compound 2; then the compound 2 is subjected to an intra-molecular cyclization reaction to obtain a compound 3; the compound 3 is subjected to a double bond hydrogenation reduction to obtain a compound 4; and the compound 4 is hydrolyzed to obtain a compound 5. The response equations are described as follows.

The invention discloses a method for synthesizing a compound ticagrelor and a synthesized intermediate thereby. The method comprises the following steps: carrying out a substitution reaction between a compound (2) and a compound (3) to prepare a compound (4); carrying out a reduction reaction on the compound (4) to prepare a compound (5); carrying out a chlorination reaction on the compound (5) to prepare a compound (6); carrying out a substitution reaction between the compound (6) and a compound (7) to prepare a compound (8); and finally, carrying out a hydroxyl deprotection reaction on the compound (8), thereby obtaining the ticagrelor (1). The reaction formulas are as shown in the specification. The invention provides a novel method for synthesizing ticagrelor. The synthetic method has the advantages of novel technical route, simple and convenient operation, high synthesis yield, high product purity, cheap and readily available raw materials and the like, and is suitable for industrialized production. Meanwhile, the synthesized ticagrelor intermediate provides a novel intermediate raw material for preparation of the ticagrelor.

The invention relates to a method for synthesizing (3aS, 6aR)-5-(tert-butoxycarbonyl)-2-oxooctahydropyrrolo[3, 4-b]pyrrole-3a-carboxylic acid, and mainly solves a technical problem of absence of a method suitable for industrial synthesis at present. The method provided by the invention comprises the following four steps: step one, dissolving a compound 1, ethyl bromoacetate and tetrabutylammoniumfluoride in tetrahydrofuran to obtain a compound 2; step two, dissolving the compound 2, hydroxylamine hydrochloride and sodium bicarbonate in a mixed solvent of tetrahydrofuran and ethanol to obtaina compound 3; step three, adding the compound 3, Raney nickel and ammonia water into ethanol, filtering and spin-drying to obtain a compound 4 after finishing reaction; and step four, adding the compound 4 and sodium ethoxide into ethanol, performing reflux reaction to obtain a white solid compound 5, namely, (3aS, 6aR)-5-(tert-butoxycarbonyl)-2-oxooctahydropyrrolo[3, 4-b]pyrrole-3a-carboxylic acid.

The invention relates to a preparation method of tert-butyl 2-iodomethyl-1-oxa-7-azaspirane [3,5] nonane-7-carboxylic ester and mainly solves the technical problem that no appropriate industrial synthesis method exists at present. The method comprises two steps as follows: firstly, a compound 1 and a compound 2 produce a compound 3 under the action of zinc powder and ammonium chloride, then the compound 3 reacts with iodine and sodium bicarbonate in acetonitrile, a compound 4 is obtained, and the equation is shown in the specification. The compound obtained with the method is a useful intermediate for synthesis of numerous drugs or product.

The invention relates to a preparation method of 1-benzyl-8-tert-butyl-2-hydroxymethyl-1,8-diazaspirane[4.5]decane-1,8-dicarboxylate, mainly aiming at solving the technical problem that a suitable industrial synthesis method does not exist at present. The preparation method comprises six steps: firstly, taking a compound 1 and oxalyl chloride to react in dichloromethane, so as to generate a compound 2; then obtaining a compound 3 under the action of triethylamine; then taking the compound 3 to react with a vinyl Grignard reagent, so as to obtain a compound 4; then taking the compound 4 and a compound 5 to react under the condition that DBU is used as alkali, so as to obtain a compound 6; carrying out hydrogenation ring closure to obtain a compound 7; finally, taking the compound 7 to react with benzyl chloroformate under an alkaline condition, so as to obtain a final product 8. The compound prepared by the preparation method is used as a useful intermediate or product for synthesizing various medicines.

The invention relates to a preparation method of (3aR, 7S, 7aR)-tertiary butyl 7-hydroxyhexahydrofuro-[3,2-b] pyridine-4(2H)-carboxylic ester, and mainly solves the technical problem of no method suitable for industrial synthesis currently. The preparation method disclosed by the invention comprises nine steps in total; in the ninth step, under the action of sodium borohydride, a pair of compounds 12 and 12A are obtained. ( The structural formulas of the compounds are shown in the description) The compounds obtained by the preparation method are useful intermediates or products synthesized by various medicaments.

The invention relates to a preparation method of 3-(difluoromethoxy) piperidine hydrochloride. The main technical problem is solved that in the prior art, no suitable industrialized synthesis method exists. The preparation method comprises the two steps that in the first step, a compound 1 is added into acetonitrile, copper iodide is added into a solution, a mixture is heated, then 2-(fluorosulfonyl) difluoroacetic acid, and after a reaction is ended, a compound 2 is obtained through purification of after-treatment; in the second step, the compound 2 is stirred in an ethyl acetate hydrochloride solution to obtain a compound 3, wherein the reaction formula is shown in the specification. The obtained compound is an intermediate or a product which is synthesized by many medicines.

The invention relates to a preparation method of 8-tert-butyl-1-ethyl-6,7-dihydro-5H-imidazo[1,5-a][1,4]diazepine-1,8(9H)-dicarboxylic acid ester. A purpose of the present invention is to mainly solvethe technical problem that no suitable industrial synthesis method exists at present. According to the present invention, the method comprises nine steps, the synthetic route is defined in the specification, and the obtained compound can be used as the useful intermediate or product for synthesizing a plurality of medicines.

The invention discloses a synthesis method of a ticagrelor intermediate. The method comprises the steps of allowing a compound (2) and a compound (3) to perform a coupling reaction to form a compound (4), and allowing the compound (4) to perform a rhodium-catalyzed asymmetric ternary cyclization reaction to form a ticagrelor intermediate compound (1), wherein a reaction formula of the method is shown in the description. The synthesis method has the advantages that the method is novel in technical route, easy and simple to operate, high in synthesis productivity and suitable for industrial production, a product is high in purity, and raw materials are cheap and easy to obtain. The compound (1) prepared by the rhodium-catalyzed asymmetric ternary cyclization reaction is a novel catalytical system; the novel system has the characteristics of mild reaction conditions, simple post-treatment, lower overall cost, relatively easy amplification of the reaction and the like; at the same time, the synthesized ticagrelor intermediate provides an intermediate raw material for preparation of ticagrelor and serves as an important intermediate for synthesis of ticagrelor.

The invention relates to a preparation method of tertiary butyl-1-methyl-5-oxysub unit triazaspiro[5.5] undecane-8-formyl ester and primarily solves the technical problem that proper industrial synthetic methods are not available in the prior art. The preparation method comprises two steps: S1, adding ethanediamine and benzyl triethyl ammonium chloride by taking dichloromethane as a solvent, reducing the temperature of a reaction system to 5 DEG C and dropwise adding an aqueous solution of sodium hydroxide, stirring the mixture to react, dissolving N-Boc-3-piperidone and chloroform in dichloromethane into the reaction system when the temperature of the system is raised to 10 DEG C, and stirring the mixture to react when the reaction temperature is 15 DEG C to obtain a compound 3; and S2, dissolving the compound 3 in methanol at room temperature, adding formaldehyde and acetic acid, reducing the temperature of the reaction system to 0 DEG C, adding sodium cyanoborohydride, and carryingout a reaction at 20 DEG C and carrying out purification treatment to obtain a final product. The compound obtained by the invention provides an important intermediate for synthesizing many drugs.