46 results about "Methylene Dichloride" patented technology

The invention relates to the technical field of organic synthesis, in particular to a method for constructing Orforglipron pyran ring chirality through enzyme catalysis, which comprises the following steps: step S1, taking SM1 and SM2 as raw materials, and reacting under the action of a palladium catalyst and a ligand to obtain INT-1; step S2; carrying out hydrogenation reduction on double bonds of the INT-1 under the catalysis of Pd / C to obtain INT-2; s3, carrying out hydrolysis resolution on the INT-2 in a solvent, a buffer salt system and enzyme catalysis to obtain a chiral pure intermediate INT-3; step S4, performing ring closing on the INT-3 through a Grignard reaction to synthesize a lactone intermediate INT-4; and S5, carrying out Diball-H reduction, quenching, dichloromethane extraction and anhydrous sodium sulfate drying on the INT-4, and then reducing by using triethyl silane to obtain the compound with the general formula A. Chirality is constructed through enzyme catalysis, isomer impurities do not need to be split and separated through SFC when the chirality is constructed, loss is reduced, the yield is increased, and a target product is obtained with high yield and high chiral selectivity; meanwhile, the cost is relatively reduced, and the cost is saved.

The invention relates to the technical field of cefuroxime sodium medicines, and in particular provides a method for recycling a cefuroxime sodium mother liquor. On the basis of the prior art, a mother liquor nanofiltration impurity removal step and an organic solvent permeation steam recovery step are added, and cefuroxime acid and organic solvents acetone, ethyl acetate and dichloromethane in the cefuroxime sodium mother liquor can be effectively recycled and utilized, which not only solves the heavy environmental burden for production enterprises, but also brings potential considerable economic benefits to the production enterprises, and has great economic value and social value.

The preparation method comprises the following steps: crushing epimedium sagittatum to prepare paste, suspending with water, extracting with petroleum ether, dichloromethane, ethyl acetate and n-butyl alcohol respectively to obtain extractum of each part, carrying out gradient elution separation by using silica gel column chromatography, and concentrating to obtain the isopentenyl flavone compound extracted from epimedium sagittatum, thereby obtaining the isopentenyl flavone compound extracted from epimedium sagittatum. Combining the similar parts according to a thin layer chromatography (TLC) color development result to obtain a plurality of polar segments; carrying out chromatography and gradient elution on the target polar section to obtain a plurality of components, and then combining the similar components through thin-layer chromatography (TLC) dot plate absorption to obtain a plurality of sub-components; a target component is eluted and purified, fractions with different retention times are collected and dried, and two compounds are respectively obtained, have a remarkable inhibition effect on the cell viability of human breast cancer cells MCF-7, have anti-breast cancer activity, can be applied to preparation of drugs for treating breast cancer, and have huge social and economic benefits.

The subject of the invention is N-substituted derivatives of l-(l-phenyl-3-aryl)-lH-pyrazol-4-yl)methanamine with the general formula 1, where ¥ represents CH or N, R1 represents hydrogen, R2 represents no substituent, R3 represents hydrogen, while R4 represents N-propylbenzamide, benzo[b]furan, dihydrobenzo [b] furan, methylenedioxybenzene, ethyl benzoate, or propyl benzoate, substituted accordingly, their method of production and application, and the method of obtaining and application of N-substituted derivatives of l-(l-phenyl-3-aryl)-IH-pyrazol-4-yl)methanamine with the general formula 1, where Y represents C, CH, or N, R1 represents hydrogen or a methyl group, R2 represents a methyl group or no substituent, R3 represents hydrogen or a methyl group, while R4 represents dimethylpyrazole, methylpyrazole, dimethylimidazo[l,2-a]pyrimidine, or isopropoxybenzene, substituted accordingly. The compounds that are the subject of the invention are obtained through reductive amination using borohydride derivatives as the reducing agent, advantageously sodium triacetoxyborohydride, in the amount of 1.4-2.0 eq, amine in the amount of 1.0-1.1 eq, advantageously in slight excess, base, advantageously triethylamine in the amount of 1.0-1.1 eq (in the case of using amine in the form of hydrochloride), and the starting aldehyde. The reaction is conducted in a nonpolar solvent environment, advantageously dichloroethane at a concentration of about 0.1 M. The crude product is purified by column chromatography on silica gel using a methanol in dichloromethane mixture as the eluent, in concentration ranges from 2% to 5%. In order to obtain a solid form and improve the physicochemical parameters, the free bases are converted into hydrochloride form, and then crystallized from a polar solvent, advantageously ethanol or propanol.

The invention relates to a green synthesis method of triphenylphosphine, which belongs to the technical field of organic synthesis, and comprises the following steps: Step 1: adding a solvent, benzene and a catalyst aluminum trichloride into a reaction flask, heating to 25-30 DEG C, dropwise adding phosphorus oxychloride, after addition, carrying out heat preservation reaction, and after the reaction is finished, cooling to room temperature to obtain a reaction product; the heat preservation temperature is 25-30 DEG C, and the heat preservation time is 3-4 hours; 2, after the reaction is finished, water is added for washing and layering, an organic phase is concentrated, the solvent is recycled, and triphenylphosphine oxide is obtained; 3, reducing the triphenylphosphine oxide in a solvent through a reducing agent to obtain triphenylphosphine, wherein the reducing agent is a triethyl silane / oxine copper reduction system; and Step 4, after the reaction is finished, cooling to room temperature, adding water for washing and layering, concentrating an organic phase, and recovering the solvent to obtain the triphenylphosphine. The synthesis method is safer and more environment-friendly, the greenization of the process is embodied, the safety and environmental protection pressure is greatly relieved, the technological process is simple, the yield is high, and the synthesis method is suitable for industrial large-scale production.

The invention belongs to the technical field of biomedicine synthesis, and particularly relates to the technical field of chemical synthesis of natural drugs / prodrugs for controlling metabolic abnormalities such as blood sugar and blood fat. The invention provides a preparation method of a cholic acid derivative. The preparation method comprises the following steps: adding benzyl bromide into an alkaline solution containing cholic acid to obtain benzyl cholate; the method comprises the following steps: adding a dichloromethane solution containing acyl chloride into a dichloromethane solution containing benzyl cholate and 4-dimethylaminopyridine under protective gas to obtain a colorless oily product; and introducing hydrogen into the absolute ethyl alcohol in which the colorless oily product is dissolved to obtain the cholic acid derivative. The chemical synthesis of the cholic acid derivative is realized.

The invention relates to the technical field of pharmaceutical engineering, in particular to a fluorouracil production process which specifically comprises the following condensation reaction steps: S1, adding a base catalyst into dichloromethane, and dropwise adding ethyl formate and ethyl fluoroacetate to obtain a mixture, the mass of the dichloromethane is 3-7 times that of the ethyl fluoroacetate, and the molar equivalence ratio of the added base catalyst to the ethyl formate to the ethyl fluoroacetate is (2.5-3.5): 2.5: 1; s2, controlling the temperature of the mixture obtained in S1 to 30-40 DEG C, and continuously stirring to react for 0.5-2 hours to obtain an intermediate state substance; according to the production process of the fluorouracil, provided by the invention, the production cost during mass production can be remarkably reduced, and meanwhile, the quality and the stability of the fluorouracil product are ensured.

A method for producing α-amino acid poly(ester amides), poly(ester ureas), and copolymers thereof by interfacial polycondensation comprises the following steps: (a) preparing a first solution by mixing bis(α-amino acid)-, ω-alkylene diester di-p- toluenesulfonate salt, and anhydrous sodium carbonate in water; (b) preparing a second solution by dissolving an aliphatic dicarboxylic acid chloride, or triphosgene, or a mixture of triphosgene with aliphatic dicarboxylic acid chlorides and / or a mixture of triphosgene with aliphatic diisocyanates in methylene chloride; (c) cooling both the first and the second solutions; (d) adding the second solution to the first at a rate of 2350–2400 mL / min under stirring at 680–700 rpm; (e) adding 4.0–4.5 L of distilled water to the resulting reaction mixture in the reactor; (f) adding 10–12 L of distilled water to the polymer solution in the distillation / washing unit while simultaneously performing azeotropic distillation of methylene chloride and washing the polymer; and (g) drying the obtained polymer.

This invention provides a composition that inhibits the tyrosinase enzyme involved in melanin production and also inhibits the action of collagen-degrading enzymes, thereby promoting collagen synthesis and achieving sufficient effects of skin whitening and elasticity improvement without inducing skin irritation due to skin allergies. [Solution] A composition having skin whitening and skin elasticity improving effects, according to one embodiment of the present invention, contains ginger extract as an active ingredient, and the ginger extract can be extracted using methylene chloride.

To efficiently increase a production ratio of carbon tetrachloride when methyl chloride is reacted with chlorine to produce higher chlorinated methanes consisting of methylene chloride, chloroform, and carbon tetrachloride.SOLUTION: In a method for producing higher chlorinated methanes, chlorination reaction is carried out in such a manner that at least a part of chloroform contained in highly chlorinated methanes is separated and circulated and supplied to the reaction system of the highly chlorinated methanes, while the methylene chloride contained in the higher chlorinated methanes is circulated and supplied to the reaction system in an amount ranging from 0 to 100 mass% relative to chloroform being circulated and supplied to the reaction system.SELECTED DRAWING: Figure 1

The utility model relates to the technical field of gas collecting devices, in particular to a dichloromethane adsorbing and collecting device which comprises a heating kettle, a reaction container, a waste liquid collecting bottle, a low-temperature cooling circulating pump, a cold trap and a vacuum bottle, the heating pot is used for heating a reaction container containing a mixture; the reaction container is connected with a gas inlet of the waste liquid collecting bottle; a gas outlet of the waste liquid collecting bottle is connected with a gas inlet of the cold trap; the cold trap is arranged in a thermos bottle filled with dry ice; the low-temperature cooling circulating pump is connected with the waste liquid collecting bottle and is used for cooling the waste liquid collecting bottle. Heating the mixture through a heating pot to generate dichloromethane gas, and then carrying out primary liquefaction and collection on the dichloromethane gas in a waste liquid collection bottle; carrying out secondary liquefaction on the dichloromethane gas in the cold trap and collecting the dichloromethane gas; in the secondary liquefaction process, the cooling temperature of the dry ice is lower than the liquefaction temperature of the dichloromethane, and the liquefaction effect on the dichloromethane is better.

The polyarylester emulsion post-treatment equipment comprises a reaction table, a water bath cavity is formed in the middle of the reaction table, a glass reaction kettle is fixedly installed in the middle of the water bath cavity, a tank cover assembly matched with the glass reaction kettle is arranged on the glass reaction kettle, and a main supporting column is fixedly arranged on one side of the top end of the reaction table; according to the polyarylester emulsion post-treatment equipment and the novel treatment process thereof, the process is environmentally friendly, the cost is low, operation is easy, a large amount of methanol organic solvent does not need to be poured in the treatment process for demulsification, and only direct distillation recycling treatment is conducted in an original sealed reaction kettle; according to the method, the low-boiling-point reaction solvent dichloromethane can be obtained by using the methanol demulsification process, the use of a large amount of methanol organic solvent in the methanol demulsification process and the subsequent separation of the methanol and dichloromethane mixed solvent are omitted, the methanol solvent volatilized into the environment is also greatly reduced, and the environment and experiment operators are protected.

The invention belongs to the technical field of synthetic chemistry, and particularly relates to a preparation method of a high-chiral-purity suvorexant intermediate. The preparation method comprises the following steps: by taking (5R)-hexahydro-5-methyl-1-benzyl-1H-1, 4-diazepine as an initial raw material, triethylamine as alkali and dichloromethane as a solvent, carrying out BOC acid anhydride protection to obtain an intermediate 1; dissolving the intermediate 1 in methanol, catalyzing by palladium carbon, and removing benzyl protection to obtain an intermediate 2; performing CBZ protection on the intermediate 2 under an alkaline condition to obtain an intermediate 3; and removing BOC protection from the intermediate 3 under an acidic condition to obtain the suvorexant intermediate with high chiral purity. The synthesis process is simple, the yield is high, the chiral purity reaches 99.8% or above, the solvent and the catalyst can be recycled, and the method is green and environmentally friendly.

The utility model belongs to the technical field of methylene methyldisulfonate production, and particularly relates to a methylene methyldisulfonate production system which comprises an esterification kettle, an extraction tank, a primary centrifugal machine, a crystallization kettle, a secondary centrifugal machine and a spiral conveyor which are sequentially connected, and the top of the extraction tank and the top of the crystallization kettle are both connected to a dichloromethane elevated tank; the top of the extraction tank is further connected to a tube pass upper opening of the condenser through a pipeline, a tube pass lower opening of the condenser is connected to a liquid inlet of the esterification kettle through a pipeline, a liquid discharging opening of the primary centrifugal machine is connected to a primary mother liquor tank, and a liquid discharging opening of the secondary centrifugal machine is connected to a secondary mother liquor tank. The production system is reasonable in structural arrangement, methylene methyldisulfonate in the esterification liquid is extracted by using dichloromethane instead of water, the output of wastewater is greatly reduced, severe heat release is avoided in the treatment process, and the safety risk is greatly reduced.

This invention provides a composition that inhibits the tyrosinase enzyme involved in melanin production and also inhibits the action of collagen-degrading enzymes, thereby promoting collagen synthesis and achieving sufficient effects of skin whitening and elasticity improvement without inducing skin irritation due to skin allergies. [Solution] A composition having skin whitening and skin elasticity improving effects, according to one embodiment of the present invention, contains ginger extract as an active ingredient, and the ginger extract can be extracted using methylene chloride.

The invention discloses a method for preparing an alpha-hydroxyl ester compound by utilizing lignite residue catalysis, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: S1, mixing water and an aryl diazo ester compound, then adding acetonitrile in an air atmosphere, and stirring; s2, adding lignite residues as a catalyst to catalyze a reaction, reacting at room temperature for 1 h, heating to 80 DEG C, and continuously reacting for 8-10 h; s3, stopping the reaction when the reaction is detected to be complete by TLC; and S4, filtering the reaction liquid, washing a filter cake with dichloromethane until the filter cake is colorless, carrying out reduced pressure concentration on the filtrate to remove volatile components, and carrying out silica gel column chromatography separation to obtain the alpha-hydroxyl ester compound. According to the method, the lignite residues are used as the catalyst which is wide in source, low in cost and easy to obtain, and other transition metals or complex ligands do not need to be additionally introduced in the reaction; the reaction conditions are mild, the yield is good, gram-scale reaction can be realized, and the method has industrial prospects; meanwhile, waste resources can be recycled, and the development themes of green chemistry and green environmental protection are met.

The present application relates to a kind of preparation methods of waste tobacco extract, waste tobacco is crushed, enzymolysis, organic solvent ultrasonic extraction obtains methylene chloride extract S1 and ethyl acetate extract S2;After enzymolysis treatment, tobacco powder is fermented, subcritical water extraction, heavy metal adsorption and nanofiltration membrane filtration, nanofiltration membrane permeate is concentrated to obtain concentrated extract, concentrated extract is carried out molecular distillation, the light component and heavy component of molecular distillation are collected, the light component is water extract S3, and the heavy component is water extract S4;Concentrated extract is obtained by concentrating the cut-off liquid, and is recorded as water extract S5;The waste tobacco extract is one or more than two of methylene chloride extract S1, ethyl acetate extract S2, water extract S3, water extract S4 and water extract S5.The extract contains a large amount of tobacco native substance, has strong tobacco style characteristics, and higher safety, and it is applied to cigarette, can significantly improve the sensory quality of cigarette.

The present invention relates to the technical field of extraction method of hypocrellin, and in particular to a method for preparing high-purity hypocrellin. The method includes adding sodium chloride aqueous solution to hypocrellin crude extract and stirring, adding dichloromethane for extraction, adding sodium hydroxide aqueous solution to the extract and stirring, standing, and layering, separating and removing the aqueous phase, and then repeatedly adding sodium hydroxide aqueous solution, collecting hypocrellin extract after separation; decompression and recovery of dichloromethane, concentrating the hypocrellin extract to a paste, washing the paste with petroleum ether, filtering, and drying, to obtain; or, concentrating the hypocrellin extract to a solid content of 40wt%-80wt%, standing and crystallizing, washing the crystals with petroleum ether, and drying, to obtain. The purity of hypocrellin obtained by the method of the present invention can reach 99.9%, and the method of the present invention greatly reduces the preparation cost of high-purity hypocrellin, and is suitable for large-scale production of high-purity hypocrellin.

The invention relates to the technical field of biopesticides, in particular to application of tobacco root exudate extract in prevention and treatment of aphid diseases of Chinese roses, tobaccos, wheat and cruciferous vegetables, and a preparation method of the tobacco root exudate extract comprises the following steps: extracting tobacco root exudate by adopting a solvent, and concentrating to obtain the tobacco root exudate extract; the solvent is ethyl acetate or dichloromethane; the volume ratio of the solvent to the tobacco root exudates is (0.5-1.5): 1. According to the invention, the dichloromethane extract of the tobacco root exudates is used for preventing and treating the plant aphids for the first time, the extract can effectively kill and inhibit the plant aphids, and the insecticidal activity rate of the extract on the plant aphids is gradually increased along with the increase of the concentration of the extract of the tobacco root exudates. The tobacco root exudates are derived from plants, are easy to degrade in nature, are safe to the environment, and do not pollute grains, and pests are not easy to generate drug resistance.

The invention relates to the technical field of film production, and discloses a liquid scraping roller on-line automatic roller wiping device which comprises a groove body, a mounting main shaft is arranged on the inner wall of the groove body, a liquid scraping roller is fixed to the mounting main shaft through a mounting base, the mounting base is connected with a sliding rod base, and a sliding rod is arranged at the end, away from the mounting base, of the sliding rod base. According to the online automatic cleaning device for the liquid scraping roller, the function of instantly cleaning the roller surface during production of a production line is achieved, shutdown for use is not needed, the cleaning device is simple in structure and convenient to operate, the production efficiency is improved, and the production cost is reduced. And through the mechanical automatic cleaning function, the danger caused by manual online cleaning is reduced, cleaning personnel are prevented from being in direct contact with the washing liquid, and the harm of dichloromethane to the human body is prevented.

The invention belongs to the technical field of chemical pharmacy, and particularly relates to a preparation method of high-purity landiolol hydrochloride, which comprises the following steps: mixing a landiolol hydrochloride crude product and a benign solvent, decolorizing, filtering, adding a poor solvent into the filtrate, crystallizing, and filtering to obtain the landiolol hydrochloride, the benign solvent is one or more of dichloromethane, ethyl acetate, absolute ethyl alcohol, methanol, dimethyl sulfoxide and N, N-dimethylformamide, and the poor solvent is one or more of normal hexane, cyclohexane, methylbenzene and petroleum ether; the invention has the advantages of higher purity and fewer impurities.

The invention relates to the technical field of medicines, and discloses a refining method of tretinoin, which comprises the following steps: S1, dissolving a tretinoin crude product with a mixed solvent of dichloromethane and lower alcohol, adding activated carbon for decoloration, and filtering; and S2, distilling the filtrate obtained in the step S1, adding low alcohol in the distillation process for band removal, then cooling and crystallizing, washing crystals with low alcohol, filtering, and drying to obtain refined tretinoin. According to the refining method, the influence of impurities in the crude product can be avoided, a good technical effect is achieved, the purity of tretinoin reaches 99.9% or above, the single impurity content is not higher than 0.05%, the total impurity content is lower than 0.1%, the refining yield reaches 90% or above, and the refining method is suitable for industrial production.

The utility model belongs to chemical organic synthesis equipment technical field discloses a kind of synthesis device of methyl acetate, reaction kettle, plate and frame filter press, distillation kettle, stainless steel condenser, product receiving kettle, methylene chloride receiving kettle and vacuum pump;The outlet valve of the bottom of the reaction kettle is connected to the inlet end of the plate and frame filter press by pipeline;The outlet end of the plate and frame filter press is connected to the inlet end of the distillation kettle by pipeline;The outlet end of the top of the distillation kettle is connected to the inlet end of the stainless steel condenser by pipeline;The outlet end of the stainless steel condenser is connected to T type control valve;The first outlet end of the T type control valve is connected to the inlet end of the methylene chloride receiving kettle by pipeline;The second outlet end of the T type control valve is connected to the inlet end of the product receiving kettle by pipeline;The inlet end of the top of the product receiving kettle is connected to the vacuum pump by pipeline.

The invention discloses a separation and purification method of erythromycin-6,9-imidoether, and erythromycin-6,9-imidoether is separated and purified by three-stage countercurrent centrifugal extraction technology and composite solvent crystallization technology. Erythromycin oxime salt is freed with a hydrophobic solvent, and extraction and separation are performed by three-stage countercurrent centrifugal extraction technology, that is, the free extraction time is shortened, and erythromycin oxime is prevented from being too long under alkaline conditions, and degradation occurs and affects product quality. Composite solvent crystallization technology is used for purification, that is, the residue of hydrophobic solvent dichloromethane in the reaction solution can be effectively removed, and erythromycin-6,9-imidoether can be directly purified and extracted, while replacing the refining process of ethanol and acetone in the traditional process, so as to achieve the purpose of reducing production costs and improving product yield.

The invention discloses a method for synthesizing β-aminoketone compounds by titanocene / Brønsted acid synergistic catalysis, using dichlorodiphenyltitanate as a Lewis acid catalyst, 2,3-quinolinedicarboxylic acid as an acid ligand, and dichloromethane as a solvent, and using a one-pot method to make aromatic aldehydes, aromatic amines and cyclohexanone three components carry out carbonyl protonation, amines undergo nucleophilic addition to carbonyl groups, deprotonation, electron transfer on nitrogen, and water departure at room temperature to obtain an iminium ion intermediate; iminium ions, as electrophilic reagents, attack the enol structure containing active hydrogen compounds, lose protons, and obtain β-aminoketone compounds. The present invention has low cost, extremely mild reaction conditions, simple operation, short reaction time, high selectivity of catalysts, and the product only needs simple column chromatography separation after the reaction is completed. The synthesized β-aminoketone compounds have diverse biological and pharmacological activities.

An anion exchange membrane is made by mixing 2 trifluoroMethyl Ketone [nominal] (1.12 g, 4.53 mmol), 1 BiPhenyl (0.70 g, 4.53 mmol), methylene chloride (3.0 mL), trifluoromethanesulfonic acid (TFSA) (3.0 mL) to produce a pre-polymer. The pre-polymer is then functionalized to produce an anion exchange polymer. The pre-polymer may be functionalized with trimethylamine in solution with water. The pre-polymer may be imbibed into a porous scaffold material, such as expanded polytetrafluoroethylene to produce a composite anion exchange membrane.

The present invention discloses a curcumin based spray bandage formulation that includes 95% Curcuma longa IH 4 % w / w, isopropyl alcohol 383 % w / w, polyvinyl polymer 2.8 % w / w, castor oil 0.4 % w / w, methylene chloride 17.3 % w / w, perfume 0.2 % w / w, and propellant 37 % w / w. Also disclosed is a process for preparation of the curcumin based spray bandage formulation. The spray bandage formulation of the present invention is applied by spraying from an aluminum can directly onto a wound to form an antiseptic waterproof spray bandage. The spray bandage formulation enhanced with the healing properties of curcumin, forms a protective layer resembling natural skin, and effectively treats by shielding the wounds, cuts, and abrasions from infections. The spray bandage formulation disappears from the wound upon healing, and hence prevents the problems associated with removal of a bandage.

The invention discloses a polyethylene glycol linker for protein modification, with a chemical structural formula of #imgabs0#. The synthesis method thereof includes: S1: synthesis of compound 2; S2: synthesis of compound 3; S3: synthesis of compound 4; S4: synthesis of compound 5; S5: synthesis of compound 6: dissolving pentafluorophenol activated ester in dichloromethane, adding compound 5 synthesized in the above steps, and after complete reaction at room temperature, adding water to the reaction solution, extracting, washing with water, and pulling through a column to obtain compound 6. The synthesis method of the polyethylene glycol linker for protein modification has easy-to-obtain raw materials, simple operation, and low cost. The polyethylene glycol linker prepared has a thiol group at one end and a biotin group at the other end, which is convenient for utilizing the thiol group and the protein linker to modify the monomer of the nanoliposome preparation material, thereby conveniently introducing the biotin group on the surface of the protein or the nanoliposome particle.