15 results about "Acetonitrile" patented technology

The invention discloses a method for preparing a 2-iodine amyl -2-ene-1,4-diketone derivative by adopting visible light catalysis. The method comprises the steps of adding allene, perfluorobutyl iodide, an additive and a photocatalyst as shown in a formula (I) to an organic solvent at the molar ratio of 1:(1-2):(1-2):(0.005-0.1), stirring under the conditions of an oxygen atmosphere, visible light illumination, room temperature and ordinary pressure for 10-20h, carrying out post-treatment on a reaction liquid to obtain a 2-iodine amyl -2-ene-1,4-diketone derivative as shown in a formula (II), wherein the additive is NaI, NH4I or KI; the organic solvent is ethanol, dichloromethane, benzene, methylbenzene, tetrahydrofuran or acetonitrile; the photocatalyst is selected from one of the following components: Ir(ppy)3, Eosin Y, Rose Bengal, [Ir(dF-CF3-ppy)2(dtbbpy)]PF6, [Ir(ppy)2(tbbpy)]PF6, Ru(bpy)3(BF4)2. The method is mild in reaction condition, simple in operation, high in selectivity and good in yield; a substituent group can be expanded; and visible light catalysis is adopted, so that the method has the characteristics of being free of pollution and environment-friendly. The formulas are as shown in the specification.

The invention discloses a method for preparing oxiracetam (4-hydroxylethylpyrrolidone-2-acetamide) used for improving brain functions. The method comprises the following steps: taking chloroacetoacetic ester and aminoacetonitrile hydrochloride (aminoacetonitrile sulphate) as raw materials, and conducting the steps such as hydrogenation, substitution, cyclization and the like on the chloroacetoacetic ester, and finally synthesizing and obtaining the objective product; and the preparation method has the advantages that the price of the raw materials is cheap and the materials are easy to obtain, the cost is low, the technical process is simple, and compared with the prior art, the yield rate is higher, the product quality is better, thus being more suitable for the industrialized scale production.

The invention discloses a refining method for high-purity bepotastine besilate. The refining method is a solvent crystallization method adopting a crude bepotastine besilate product as a raw material and comprises the following steps: firstly, the crude bepotastine besilate product is heated and dissolved with acetonitrile and filtered, a filtrate is cooled, stirred and crystallized, crystals are filtered and dried, and primary refined product is obtained; the primary refined product is heated, stirred, dissolved in water and filtered, a filtrate is cooled, stirred and crystallized, crystals are filtered and dried, and a pure bepotastine besilate product is obtained. The method has the advantages that the operation is simple and convenient, the yield is high, the product is pure, the cost is saved and the like, the total yield is 80% or higher, the purity of the pure bepotastine besilate product is 99.9% or higher proved by HPLC detection, the isomer impurity content is reduced to 0.1% or lower from 0.4%, and other single impurity content is reduced to 0.1% or lower from 0.2%.

The present invention relates to a method for preparing diphenylethanone from benzyl alcohol through a photocatalytic one-step method. According to the method, diphenylethanone is directly prepared byusing inexpensive benzyl alcohol as a raw material under the action of a solid photocatalyst; and the reaction process comprises: mixing benzyl alcohol, a catalyst and an acetonitrile solvent are mixed, placing in a pressure container, replacing with an inert gas, and carrying out illumination stirring at a room temperature, wherein the reaction time is more than 1 h, the catalyst is easily separated from the reaction system after the reaction and can be recycled multiple times, and the separation yield of diphenylethanone is up to 81%.

The invention relates to the field of production preparation of compounds, in particular to preparation and purification methods of 4-biphenylacetic acid. The preparation and purification methods comprise steps as follows: 1) biphenyl is subjected to a chloromethylation reaction to produce 4-phenyl benzyl chloride; 2) 4-phenyl benzyl chloride reacts with sodium cyanide to produce 4-biphenyl acetonitrile; 3) 4-biphenyl acetonitrile is hydrolyzed and a crude 4-bphenylacetic acid product is obtained; 4) the crude 4-bphenylacetic acid product and methanol are subjected to an esterification reaction to produce 4-biphenyl methyl acetate, 4-biphenyl methyl acetate is purified and hydrolyzed into 4-biohenylacetic acid, 4-bihenylacetic acid is refined, and a finished product is prepared.

The invention discloses a derivative based on rhodamine B and a preparation method and application thereof. The preparation method of the derivative comprises the following steps: under nitrogen protection, adding a dichloromethane solution of D-sphingol into an acetonitrile solution of N-ethyl p-toluenesulfonate of rhodamine B; in the presence of dried potassium carbonate, heating the solution tocarry out a reflux reaction to prepare a coarse product; and concentrating the coarse product and carrying out silicagel column separation to obtain a pure product. A pH titrating experiment verifiesthat in a DMSO/BR(1/99, v/v) system, the derivative does not give out fluorescence in a neutral condition, and the fluorescence intensity at 600 nm is enhanced gradually as the pH is reduced from 7.4to 2.0. The pKa value is 4.32, the pH response range is 2.0-7.4, and a golgiosome weak acidic environment is detected favorably. In addition, a probe has good selectivity, water solubility and low toxicity. An intracellular co-positioning experiment and a golgiosome pH adjusting experiment verify that the derivative can mark the golgiosome specifically in a targeted manner and can detect the pH change of the golgiosome with high sensitivity.

The invention provides long-chain soluble chitosan and a preparation method thereof. The method includes the steps that bi-bromo-hydrocarbon and N,N-dimethyl alkyl amine are mixed and then dissolved in acetonitrile, nitrogen is introduced for purification and reaction, and bromo-hyamine is obtained; then chitosan is dissolved in DMSO, nitrogen is introduced for stirring, and a chitosan solution isobtained; the bromo-hyamine is slowly added into the chitosan solution for stirring, and a crude product is obtained; and the crude product is filtered, precipitated, washed, dried and finally used for Soxhlet extraction, and a target product is obtained by drying. The prepared long-chain soluble chitosan can kill staphylococcus aureus, escherichia coli and candida albicans, and the sterilizing rate reaches 99% or above.

The invention discloses a urea [<13>C] abundance detection method. The method comprises the steps of S1, obtaining urea [<13>C] particles, grinding the urea [<13>C] particles, precisely weighing 0.5 g of ground urea [<13>C] particles, putting the urea [<13>C] particles in a 20 ml measuring flask, adding a proper amount of acetonitrile, conducting the ultrasonic treatment for 9-15 minutes, cooling to the room temperature, feeding 1 [mu]L of a test solution into a liquid chromatography-gas chromatograph-mass spectrometer, recording a generated chromatogram and the ion signal response intensities of quasi-molecular ions (12C16ON2H5+, 13C16ON2H5+ and 13C18ON2H5+, wherein the mass numbers of the above quasi-molecular ions are respectively 61.0402, 62.0435 and 64.0478, and the above quasi-molecular ions are respectively marked as A, B and C), and calculating according to the formula X=(B+C/A+B+C)*100% to obtain the abundance of urea [<13>C]. According to the technical scheme of the invention, unique chromatographic conditions and mass spectrometry conditions are adopted, so that the detection is simpler and more convenient. Meanwhile, human error factors during the detection process are reduced, so that the reproducibility of detection results is improved. Detection results are more accurate.

The invention discloses a synthesis method of an indole-2,3-dione compound. The method comprises the following steps that a raw material as shown in a formula I is added into a Schlenk reactor, then acatalyst bis(acetonitrile)dichloropalladium (PdCl2(CH3CN)2), an oxidizing agent silver acetate (AgOAc) and a solvent methylbenzene are added, reaction is carried out under an oxygen atmosphere at 120-150 DEG C for 8-36 hours, a TLC board is used for monitoring the reaction, and after the reaction is carried out completely, the indole-2,3-dione compound as shown in a formula II is obtained throughpost-treatment.

The invention discloses a method for extracting vavasu (one kind of isoflavone compounds) from Ceiba pentandra (L.) Gaertner. The method comprises the steps of taking tree barks of the Ceiba pentandra (L.) Gaertner as a raw material, crushing and then extracting the raw material in a fluid dynamic continuous countercurrent extraction device, putting the extraction solutions together to recycle ethanol, conducting purification by means of membrane separation, adsorbing by polyamide resin column on a permeation solution, eluting water and alcoholic solution, collection target components, concentrating the solution, extracting the concentrated solution by ethyl acetate, concentrating the extraction solution to a small size, standing by to crystalize the solution, recrystallizing crystals by using acetonitrile-dichloromethane, and then freezing and drying the crystals to obtain the vavasu. The process is simple in process, high in extraction efficiency and low in cost, thereby being quite beneficial to industrialized production.