36 results about "Butyrolactone I" patented technology

The invention relates to a synthetic method for glufosinate ammonium. The synthetic method comprises the following steps: single-bromine substitution, amination, amino protection, chlorination ring opening, Arbuzov reaction and acidizing hydrolysis ammoniation; the single-bromine substitution means triggering alpha-site single-bromine substitution betweengamma-butyrolactone I and bromine under theexistence of catalyst and performing reduced pressure distillation, thereby acquiring a pure intermediate II alpha-bromine-gamma-butyrolactone; phosphorus tribromide is served as the catalyst; amination means triggering amination reaction between alpha-bromine-gamma-butyrolactone II and ammonium hydroxide, and then adding hydrochloric acid and reflowing, thereby acquiring an intermediate IIIalpha-amino-gamma-butyrolactone hydrochloride. The invention has the beneficial effects: 1) low-costgamma-butyrolactone is taken as a raw material, is subjected to single-bromine substitution with bromineand then is subjected to amination reaction with ammonium hydroxide; the adopted raw materials are low-cost and easily acquired; reaction conditions are mild; operation is simple and convenient; safety is high; amplifying production is feasible; reaction yield is high; product purity is high; cost is greatly lowered; the synthetic method is suitable for industrial production.

The invention relates to a preparation method and application of a marine fungi aspergillus terreus butyrolactone compound butyrolactone-I. The invention discloses application of the marine fungi aspergillus terreus butyrolactone compound butyrolactone-I as shown in a formula (I) to preparation of medicaments for resisting to peripheral and neurogenic inflammation and resisting to neurodegenerative diseases. The formula is shown in the description. The invention finds that besides a DPPH free radical, butyrolactone-I can also well remove an ABTS free radical and an OH free radical; the marinefungi aspergillus terreus butyrolactone compound butyrolactone-I has better oxidation resistance and inflammation resistance and has better neuroprotection activity; therefore, the marine fungi aspergillus terreus butyrolactone compound butyrolactone-I has a wide application prospect in the aspect of preparing the medicaments for resisting to peripheral and neurogenic inflammation and resisting toneurodegenerative diseases. Meanwhile, by the preparation method of the butyrolactone-I, which is provided by the invention, the butyrolactone-I can be successfully prepared; the method is simple andeasy to realize large-scale production; culture conditions can also be optimized by addition of an inducer, so that yield of the butyrolactone-I is greatly improved.

Disclosed is a two-step, continuous hydrogenation process for the preparation of 3-methyl-tetrahydrofuran from alpha-methylene-gamma-butyrolactone, which comprises a first step of subjecting alpha-methylene-gamma-butyrolactone to hydrogenation to synthesize 2-methyl-gamma-butyrolactone; and the second step of hydrogenating the 2-methyl-gamma-butyrolactone formed in the first step. The above process enables the production of the objective highly-pure 3-methyl-tetrahydrofuran free from alcohol in high efficiency and high conversion through simple production steps.

The invention relates to the field of organic chemistry and in particular relates to a spiro-oxindole gamma-butyrolactone compound IV. The spiro-oxindole gamma-butyrolactone compound IV is prepared by taking an acid shown as a formula I and acetone shown as a formula II as raw materials, and taking dichloromethane as a solvent in the presence of N,N'-carbonyl diimidazole shown as a formula III, p-toluene sulfonic acid and cesium carbonate, reacting at 25 DEG C for 4h, concentrating a reaction solution, eluting by column chromatography, collecting eluting solution parts of all detected products and carrying out rotary evaporation to remove the solvent. The invention further provides a spiro-oxindole gamma-butyrolactone compound VI which is prepared by taking the acid shown as the formula I and N-substituted isatin shown as a formula V as raw materials, and taking tetrahydrofuran as a solvent in the presence of 2-(7-benzotriazole oxide)-N,N,N',N'-tetramethyluronium hexafluorophosphate and triethylamine, reacting at 0 DEG C for 6h, concentrating a reaction solution, eluting by column chromatography, collecting eluting solution parts of all detected products and carrying out rotary evaporation to remove the solvent. A synthesis method has the advantages of relatively good yield, wide substrate applicable range, simplicity and convenience for operation, moderate reaction, convenience for post-treatment and the like.

The invention discloses a chiral gamma-butyrolactone compound and a preparation method and an application of a derivative of the chiral gamma-butyrolactone compound. According to the preparation method, an aldehyde compound and 2-furanone are subjected to an organic catalytic asymmetric Michael addition reaction. The invention provides an effective method for combining chiral gamma-butyrolactone with three continuous chiral carbons to obtain the chiral gamma-butyrolactone compound with the yield of 89%, the dr of 9.2:1 and the ee of 99% and the derivative thereof. In addition, a cell activitytest is carried out on the chiral gamma-butyrolactone derivative obtained in the invention, so that the compound has an inhibition effect on proliferation of U251, Saos2, MGC803, 293T and Hela cell lines, and can be used as a broad-spectrum drug in treatment of various tumors.

The invention relates to the field of organic synthesis, and discloses a preparation method of alpha-acetyl-gamma-butyrolactone. The method comprises the following steps: (1) gamma-butyrolactone, CH3COOR1 and R2ONa are subjected to acylation reaction to obtain a material containing alpha-acetyl-gamma-butyrolactone sodium salt, and R1 and R2 are respectively independently C1-C4 alkyl; and (2) in the presence of water, the material containing the alpha-acetyl-gamma-butyrolactone sodium salt is enabled to be in contact with CO2 gas to generate neutralization reaction. The method also has the advantage of higher yield under the condition of ensuring safety, and provides convenience for large-scale production of alpha-acetyl-gamma-butyrolactone.

The present invention relates to a process for the preparation of Gamma-butyrolactones.

The invention discloses a preparation method of a racemic beta-aryl-gamma-butyrolactone compound. According to the preparation method, an arylboronic acid compound and gamma, gamma-disubstituted furanone are subjected to an organic catalytic asymmetric Michael addition reaction. According to the efficient preparation method provided by the invention, the gamma-butyrolactone compound reacts with aryl, and the racemic beta-aryl-gamma-butyrolactone compound with a yield as high as 98% is obtained. In addition, an intermediate is provided for preparation of a leukemia stem cell inhibitor with moreeffective activity.

The invention relates to the field of organic synthesis, and particularly discloses a method for preparing alpha-chloro-alpha-acetyl-gamma-butyrolactone. The preparation method comprises the followingsteps: (1) in the presence of a solvent, carrying out a salt forming reaction on alpha-acetyl-gamma-butyrolactone and at least one inorganic alkaline substance selected from NaOH, KOH, K2CO3 and Na2CO3 until a precipitate is generated, and then dissolving the precipitate to obtain a first solution; (2) carrying out a contact reaction on the first solution and chlorine to obtain a second solution;and (3) layering the second solution so as to obtain the alpha-chloro-alpha-acetyl-gamma-butyrolactone. The method has the advantages of simple operation, environmental protection, mild reaction conditions, and important practical significance.

The invention provides application of liquid sodium methoxide in synthesis of alpha-acetyl-gamma-butyrolactone and a synthesis method of the alpha-acetyl-gamma-butyrolactone, and relates to the technical field of organic synthesis. The synthesis method of the alpha-acetyl-gamma-butyrolactone comprises the following steps: (a) performing pre-acylation reaction on an acetate compound and gamma-butyrolactone; (b) adding liquid sodium methoxide into the reaction liquid in the step (a) to carry out mixed reaction; (c) after the reaction in the step (b) is finished, concentrating and collecting methanol, and transferring the concentrated reaction liquid into an acylation kettle; (d) supplementing the acetate compound into the acylation kettle for acylation reaction; (e) performing neutralizing, filtering and concentrating to obtain an alpha-acetyl-gamma-butyrolactone crude product. According to the method, liquid sodium methoxide is used for replacing solid sodium methoxide for acylation synthesis, so that liquification and sealing of feeding are realized, the on-site feeding risk is reduced, and the synthesis yield is increased to 96% or above.

The invention belongs to the technical field of catalysts, and discloses a catalyst for preparing gamma-butyrolactone through maleic anhydride liquid phase hydrogenation, a preparation method and application of the catalyst, and a method for preparing gamma-butyrolactone. The catalyst comprises the following components in percentage by weight: 20-70wt% of CuO, 25-75wt% of ZnO, 25-15wt% of SnO and2-8wt% of SiO2. The catalyst has high activity and selectivity, the conversion rate of maleic anhydride is greater than or equal to 95%, and the selectivity of gamma-butyrolactone is greater than or equal to 90%.

The rate of aminolysis of butyrolactones is predictably adjusted by attaching a substituent having a known field effect value (F) to the alpha position before reacting the substituted buytrolactone with an amine. The aminolysis product is a gamma-hydroxy amide. The resulting materials are useful as the cross-linking agents in a variety of coatings and coatings processes.

The invention discloses a preparation method of a chiral bicyclic gamma-butyrolactone compound, the chiral bicyclic gamma-butyrolactone compound is a main skeleton of many compounds and drug molecules and is an important active intermediate, for example, a natural product podophyllotoxin and a derivative thereof are widely applied to clinical treatment as an antitumor drug; wherein the vorapaxar sulfate serving as a marketed drug is also used as an initiative oral PAR-1 inhibitor. According to the present invention, through the double Michael addition reaction of gamma-dimethyl furanone and alpha,beta-unsaturated ketone catalyzed by (1S,2S)-1, 2-diphenylethylenediamine, so that the functional chiral bicyclic gamma-butyrolactone compound with the yield of 80%, the stereoselectivity of more than 20:1 and the higher value can be rapidly obtained through the one-step reaction. The method and the thought are provided for the synthesis of the drug active intermediate, so that synthesis difficulty of the compound in the current medicine research and development field is solved.

The invention belongs to the field of preparation of organic compounds. The invention provides a preparation method of DL-hydroxy selenomethionine. The method is characterized in that gamma-butyrolactone is used as a raw material, alpha-hydroxyl-gamma-butyrolactone is synthesized through alpha-bromination and hydroxylation, and then the alpha-hydroxyl-gamma-butyrolactone reacts with sodium methyl selenol to obtain the DL-hydroxyl selenomethionine. The method has the advantages of easily available raw materials, mild reaction conditions and low cost, and is suitable for large-scale preparation of DL-hydroxyselenomethionine.

The invention provides a recovery method and application of alpha-chloro-alpha-acetyl-gamma-butyrolactone layered water, and relates to the technical field of chemical engineering. The recovery method comprises the following steps: neutralizing the alpha-chloro-alpha-acetyl-gamma-butyrolactone layered water with alkali, and then evaporating water; and the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone is obtained by using the method disclosed by the invention. The method provided by the invention solves the technical problem of unsmooth operation of environmental protection facilities caused by viscous substances generated when the alpha-chloro-alpha-acetyl-gamma-butyrolactone layered water is used as wastewater for distillation desalination treatment, and achieves the purpose of recovering alpha-chloro-alpha-acetyl-gamma-butyrolactone from the layered water. The economic benefit is improved; and the operation efficiency of environmental protection facilities is improved.

The invention discloses a chiral bicyclic gamma-butyrolactone compound and application thereof, the chiral bicyclic gamma-butyrolactone compound is a main skeleton of many compounds and drug molecules, and is an important active intermediate, for example, a natural product podophyllotoxin and a derivative thereof are widely applied to clinical treatment as an antitumor drug; the vorapaxar sulfate serving as a marketed drug is also used as an initiative oral PAR-1 inhibitor. According to the preparation method disclosed by the invention, through double Michael addition reaction of gamma-dimethyl furanone and alpha, beta-unsaturated ketone catalyzed by (1S, 2S)-1, 2-diphenylethylenediamine, functional products are rapidly obtained through one-step reaction, the yield is as high as 80%, and the stereoselectivity is gt; the chiral dicyclic gamma-butyrolactone compound with a specific molecular weight of 20: 1 and a relatively high er value is prepared, then the chiral dicyclic gamma-butyrolactone compound disclosed by the invention is subjected to a cell viability test, and the tested compound has a certain effect of inhibiting tumor cell viability on U87MG, HCT116, SH-SY-5Y, Kyse-30, MV4-1 and MCF-7 cell lines.

The invention provides a marker combination for prognosis evaluation of liver cirrhosis, and the marker combination comprises (+/-)-3, 5, 5-trimethyl-1-hexanol, dichloromethane, pyridine, gamma-butyrolactone, citronellal, ethyl lactate, guaiacol, methyl linoleate, oxoglutaric acid, (+/-)-erythroisoleucine, 3-phenylpropanal and N-acetyl arylamine, and preferably, the N-acetyl arylamine is N-acetanilide. The invention also provides a method for determining the marker combination.

The invention relates to the technical field of short peptides prepared from cyclinasinensis and provides a method for preparing a cyclinasinensis oligopeptide for further improving the extraction efficiency of the cyclinasinensis oligopeptide. The method comprises the following steps: applying a binary system combined by ionic liquid EMIMBF4 and gamma-butyrolactone in a volume ratio of 1:1 to preparation of the cyclinasinensis oligopeptide, introducing a pulse electric field at low temperature of negative 50-negative 60 DEG C, and performing enzymolysis treatment under an enzymolysis condition of early optimized papain. The extraction rate of the cyclinasinensis oligopeptide is improved, and the bioactivity is improved to a certain extent.