41 results about "2 Butenoic Acids" patented technology

The invention discloses a preparation method for palbociclib (I). The preparation method comprises the following steps: performing cyclization reaction on 2-acetyl-2-butenoic acid methyl ester and malononitrile under an alkaline condition to generate 1,4,5,6-4H-2-methoxyl-4-methyl-5-acetyl-6-oxo-3-pyridine carbonitrile (II); performing substitution reaction on the intermediate (II) and cyclopentane halide (III) under the action of an acid-binding agent to generate N-cyclopentyl-1,4,5,6-4H-2-methoxyl-4-methyl-5-acetyl-6-oxo-3-pyridine carbonitrile (IV); performing condensation reaction on the intermediate (IV) and N-[5-(1-piperazinyl)-2-piperidyl]carbamidine (V)to generate 6-acetyl-8-cyclopentyl-5-methyl-2-[[5-(1-piperazinyl)-2-pyridyl]amino]-5,6-dihydropyrido[2,3-d]pyrimidine-7(8H)-ketone (VI); performing dehydrogenation reaction on the intermediate (VI) and sodium selenate to generate the palbociclib (I). The preparation method for the palbociclib has the advantages that the raw material is easy to obtain, the process is simple, high efficiency and environmental protection are achieved, and the preparation method is suitable for industrial production.

The invention provides a method for producing 2-butenoic acid, which comprises the following steps: preparing mixed feed liquid from 2-butenoic aldehyde, normal hexane and water in a weight ratio of 1:1:0.05-0.08; mounting an ejector pump on an oxidation reaction kettle for spraying the mixed feed liquid into the oxidation reaction kettle; introducing oxygen into the oxidation reaction kettle to perform a reaction under a condition that the reaction pressure in the oxidation reaction kettle is 0.1 to 0.6MPa and a condition that the temperature is 25 to 35 DEG C to obtain oxidation reaction solution; distilling the oxidation reaction, distilling the remaining 2-butenoic aldehyde under a reduced pressure, recovering the 2-butenoic aldehyde, distilling the remaining normal hexane at normal pressure and obtaining filtrate; and cooling the filtrate to -5 DEG C to 5 DEG C, precipitating, crystallizing and filtering and drying the crystals to obtain the 2-butenoic acid product. The production method has the advantages that: the reaction speed is high; the product yield is high; the energy consumption is small; and the quality of the product obtained is high.

The invention discloses a method for preparing 4-bialkoxy-phosphono-2-methyl-2-butenoic acid alkyl ester. According to the method, a compound shown in a formula A and a compound shown in a formula B have reaction to generate a compound having a general formula I. The method has the advantages that raw materials are easily available sources, reaction is stable and reliable, reaction conditions are mild, and environment-friendliness effect is achieved, and the method is very suitable for industrial production.

The invention relates to a concrete mud resisting agent based on counter-insert layer design and a preparing method. The method comprises the following steps that micro-molecule monomers, 2-butenoic acid, sodium methallyl sulfonate and hydroxyethyl methacrylate are stirred, dissolved and kept at the temperature of 70 DEG C-75 DEG C to obtain a uniform solution, then an oxidizing agent is added, and the mixture is stirred to obtain a uniform solution; a reducing agent and chain transfer agent mixture is added in a one-time mode, the mixture continues to be stirred for 2-4 h, pH is adjusted to be 8-9, and a proper amount of deionized water is added, so that the concrete mud resisting agent based on the counter-insert layer design is obtained. The method has the advantages that the prepared concrete mud resisting agent is provided with positive-charge functional group monomers, has a good ability to be adsorbed by montmorillonite clay preferentially, and can well stop polycarboxylate superplasticizer from being adsorbed between montmorillonite layers; the concrete mud resisting agent is high in adaptability, initial slump of concrete is increased, and the concrete has good workability.

The invention provides a method for producing 2-butenoic acid, which comprises the following steps: preparing mixed feed liquid from 2-butenoic aldehyde, normal hexane and water in a weight ratio of 1:1:0.05-0.08; mounting an ejector pump on an oxidation reaction kettle for spraying the mixed feed liquid into the oxidation reaction kettle; introducing oxygen into the oxidation reaction kettle to perform a reaction under a condition that the reaction pressure in the oxidation reaction kettle is 0.1 to 0.6MPa and a condition that the temperature is 25 to 35 DEG C to obtain oxidation reaction solution; distilling the oxidation reaction, distilling the remaining 2-butenoic aldehyde under a reduced pressure, recovering the 2-butenoic aldehyde, distilling the remaining normal hexane at normal pressure and obtaining filtrate; and cooling the filtrate to -5 DEG C to 5 DEG C, precipitating, crystallizing and filtering and drying the crystals to obtain the 2-butenoic acid product. The production method has the advantages that: the reaction speed is high; the product yield is high; the energy consumption is small; and the quality of the product obtained is high.

The invention discloses a preparation method of a key intermediate of palbociclib, namely 6-bromine-2-methylsulfinyl-8-cyclopentyl-5-methyl pyridino (2,3-d) pyrimidine-7(8H)-ketone. The preparation method comprises the following steps: taking deracil as a starting material, performing methylating, chlorinating and brominating to synthesize 5-bromine-4-chlorine-2-methylthiopyrimidine, then alkylating with cyclopentylamine, conducting a heck reaction with 2-butenoic acid, then conducting an intramolecular acylation reaction to synthesize 2-methylmercapto-8-cyclopentyl-5-methyl pyridino (2,3-d) pyrimidine-7(8H)-ketone, and finally reacting with NBS to prepare the 6-bromine-2-methylsulfinyl-8-cyclopentyl-5-methyl pyridino (2,3-d) pyrimidine-7(8H)-ketone. Steps of the preparation process are short, no dangerous process is used, the operation is simple and convenient, the cost of the raw materials is low, and the use requirement of people is met.

The invention discloses a beneficiation reagent for flotation of lead and zinc from lead-zinc oxide ore and a preparation method thereof. The beneficiation reagent is prepared from the following raw materials in parts by weight: 15-25 parts of diesel oil, 10-20 parts of sodium carbonate, 20-30 parts of sodium sulfide, 40-50 parts of 3, 3-dimethylbutyric acid, 13-18 parts of sulfur, 15-30 parts ofesterified xanthate, 25-45 parts of 3-amino-2 butenoic acid, 4-5 parts of quick lime and 20-24 parts of an activating agent. The beneficiation reagent has the characteristics of high separation efficiency, high yield, low consumption, simple and reliable process flow, easiness in operation and the like, is suitable for beneficiation application of the re-vulcanized and oxidized mixed lead-zinc ore, and can bring good economic benefits to the lead-zinc ore.

The invention discloses 4-(N-phenthiazine-)-carbonyl-2-butenoic acid and a preparation method thereof. A structural formula of 4-(N-phenthiazine-)-carbonyl-2-butenoic acid is as shown in the specification. The preparation method of 4-(N-phenthiazine-)-carbonyl-2-butenoic acid comprises the steps that A mol phenthiazine and B mol maleic anhydride are added to a reaction vessel; then C ml DMF (Dimethyl Formamide) is added; reaction liquid is obtained; the reaction liquid is heated to 100-155 DEG C on a condition of stirring and subjected to heat preservation; TLC (thin layer chromatography) is used for monitoring a reaction process; the reaction liquid is stirred continuously at 100-155 DEG C for 0.5h after raw material points are disappeared; a mixture is obtained, wherein the ratio of A to B to C is equal to 1:(1.0-1.3)-(400-800); after the mixture is cooled to a room temperature, the mixture is poured into water, subjected to suction filtration, washed and dried; and 4-(N-phenthiazine-)-carbonyl-2-butenoic acid is obtained. The method is easy and simple to operate; the reaction process is easy to control; post treatment is simple; and the productivity is high.

The invention relates to a method for preparing 4-(N-phenothiazine)-carbonyl-2-butenoic acid. The method comprises the following steps: adding A mol of phenothiazine and B mol of maleic anhydride into a reaction container, and then adding acetonitrile; dripping concentrated hydrochloric acid into the reaction container while stirring to get a reaction solution, increasing the temperature of the reaction solution from room temperature to 40-80 DEG C, and performing reaction for 1-2.5h while stirring to get a mixed solution, wherein A: B=2.5: (2.5-3.0); performing reduced-pressure distillation on the mixed solution to remove acetonitrile to get a concentrated solution, wherein the volume of acetonitrile in the concentrated solution is 15-20% of the volume of acetonitrile in the mixed solution; and cooling the concentrated solution to room temperature, then adding water into the concentrated solution, uniformly stirring, then performing suction filtration, washing a filter cake with water, and drying to get 4-(N-phenothiazine)-carbonyl-2-butenoic acid. According to the method disclosed by the invention, acetonitrile is adopted as a solvent, concentrated hydrochloric acid is taken as a catalyst, and the method has the advantages of simplicity and convenience in operation, short reaction time, mild conditions, simple post-treatment, low price and easiness in obtaining of raw materials and high yield.

The invention discloses a method for preparing alkyl 4,4-difluoroacetylacetate. The method has the advantages of easily available raw materials, simple process flow, safety in operation and high yield. The method comprises the following steps: (1) carrying out hydrolysis reaction on 1,1,2,2-tetrafluoroethyl ether used as a raw material and water in an acid and separating to obtain ethyl difluoroacetate and hydrogen fluoride; (2) reacting ethyl difluoroacetate obtained in the step (1) and alkyl acetate in the presence of an alkaline catalyst to obtain 1,1-difluoro-2-butenoic acid alkyl ester-2-hydroxy salt; and (3) neutralizing 1,1-difluoro-2-butenoic acid alkyl ester-2-hydroxy salt obtained in the step (2) and hydrogen fluoride to obtain alkyl 4,4-difluoroacetylacetate.

The invention discloses 4-(N-phenthiazine-)-carbonyl-2-butenoic acid and a preparation method thereof. A structural formula of 4-(N-phenthiazine-)-carbonyl-2-butenoic acid is as shown in the specification. The preparation method of 4-(N-phenthiazine-)-carbonyl-2-butenoic acid comprises the steps that A mol phenthiazine and B mol maleic anhydride are added to a reaction vessel; then C ml DMF (Dimethyl Formamide) is added; reaction liquid is obtained; the reaction liquid is heated to 100-155 DEG C on a condition of stirring and subjected to heat preservation; TLC (thin layer chromatography) is used for monitoring a reaction process; the reaction liquid is stirred continuously at 100-155 DEG C for 0.5h after raw material points are disappeared; a mixture is obtained, wherein the ratio of A to B to C is equal to 1:(1.0-1.3)-(400-800); after the mixture is cooled to a room temperature, the mixture is poured into water, subjected to suction filtration, washed and dried; and 4-(N-phenthiazine-)-carbonyl-2-butenoic acid is obtained. The method is easy and simple to operate; the reaction process is easy to control; post treatment is simple; and the productivity is high.

The invention provides a novel process, which takes substituted propiophenone and oxoacetic acid as starting raw materials, carries out condensation to obtain 3-(substituted benzoyl)-2-butenoic acid, and carries out reduction and nitrification to obtain a pimobendan intermediate 3-(substituted benzoyl) butyric acid. The method has the advantages of few steps, easy and simple operation, easy separation and purification of products, high yield and low cost, uses common reagents, and is the novel process suitable for industrialized production.

The invention belongs to the technical field of pesticide intermediates for synthesizing herbicides and particularly relates to a method for synthesizing a pesticide intermediate 2-amido-4-(O-alkylmethylphosphonyl)-2-butenoic acid and its ester. The method comprises that a compound VII and a compound VI undergo an Arbuzov reaction to produce a compound V, the compound V is hydrolyzed through an acid to produce a compound IV, the compound IV and a compound III undergo a reaction under action of a condensation reagent and a catalyst to produce a compound II and the compound II is hydrolyzed into a compound I. Compared with the existing synthesis route, the method has simple processes, high atom economy and high stereoselectivity, is environmentally friendly, realizes a low cost and has an industrial prospect. In the formula, R1 represents C1-4 alkyl; R2 and R3 represent CnH2n+1 and n is 1, 2, 3 or 4, or R2 or R3 represents -CmH2m- and m is 2 or 3; R4 represents C1-4 alkyl or C6-10 aryl; R5 represents hydrogen or C1-4 alkyl; and X represents chlorine or bromine.

The invention relates to a compound which is shown in the following structure and preparation and detection methods and application of the compound. The preparation method is characterized by comprising the steps that edaravone is dissolved in an organic solvent and then reacts with an aqueous hydrogen peroxide solution, the reversed-phase high-performance liquid chromatography is used for separating an edaravone reaction liquid, and (Z)-2-(3-methy-5-oxygen-1-phenyl-4,5-dihydro-1H-pyrazol-4-radical)-3-[(E)-phenylazo]-2-butenoic acid is prepared. In addition, the invention further provides thedetection method of the compound. The compound can be applied to an edaravone impurity reference substance, and the amount of edaravone raw material medicine and the amount of the compound of the related preparation are conveniently controlled. The compound is shown in the description.