55 results about "2-Butyne" patented technology

The invention relates to a synthesis method for 2-butene-1, 4-diol through selective hydrogenation of 2-butyne-1, 4-diol. The method includes placing butynediol aqueous solution and lead poisoned catalyst of Pd-C in an autoclave, replacing air with nitrogen and then replacing nitrogen with hydrogen, heating to 35 ~ 45degreeC with stirring, increasing pressure and maintaining under 0.6-1.7 MPa, reacting for 60 ~ 390 min, stopping stirring and providing hydrogen, cooling rapidly and venting, replacing unreacted hydrogen with nitrogen , and obtaining the final product for sampling analysis after filtering to remove catalyst. The quality content of catalyst is 5 wt.% Pd-C, which is poisoned by 1 -3 wt.% lead poisoning catalyst. The amount of the catalyst is 0.33 ~ 0.99 wt.% of the total reaction products. The products of this invention is a multifunctional compound, which can be formed oxygenated heterocycle after closing loop and used as the intermediates for vitamin B6 and furan ring-containing drug. Therefore, butynediol production has good market prospects.

The invention discloses a synthesis method of a trajenta intermediate. The synthesis method comprises the following steps: reacting 1-methyluracil, urea, propiodal and an oxidant under the catalytic action of acid to obtain a compound shown as a formula I; then carrying out substitution reaction on the compound shown as the formula I and 1-bromo-2-butyne to obtain a compound shown as a formula II,namely the trajenta intermediate. The method disclosed by the invention has the advantages of easily-obtained raw materials, few steps, higher yield, mild reaction conditions and suitability for industrial production. (Refer to Description).

The invention discloses a simple preparation method of II-type antidiabetic drug linagliptin which comprises the following steps: adding 3-methyl-7-(2-butyne-1-yl)-8-bromo-xanthine into a DMSO (dimethylsulfoxide) solution of 2-chloromethyl-4-methyl-quinazoline and potassium carbonate A, and under the catalysis of potassium iodide, reacting for 7-8 hours at a temperature of 70-80 DEG C; adding potassium carbonate B and (R)-3-aminopiperidine, and reacting for 7-8 hours at a temperature of 70-80 DEG C; after the reaction is completed, adding saturated salt water, separating out solids, and carrying out suction filtration to obtain a crude product linagliptin; and recrystallizing the crude product linagliptin with methyl alcohol, carrying out suction filtration and drying, thus obtaining a target product. The method disclosed by the invention is implemented by using a one-pot method, so that the method is simple and easy to operate and short in reaction steps, and raw materials are cheap and easily available, therefore, the method is applicable to industrial mass production; and the method overcomes the problems in the conventional method that impurities are difficult to remove, line operations are complicated and time-consuming, and too many raw materials are required.

The invention belongs to the technical field of organic chemical industry, and particularly relates to a method for removing 2-butyne by conducting selective hydrogenation on C5 fractions. The method particularly comprises the following steps of 1 denitrification, wherein denitrification treatment is conducted on the C5 fractions through a fixed bed containing sulfonic group cation exchange resin and water; 2 selective hydrogenation, wherein selective hydrogenation is conducted on the C5 fractions obtained after denitrification through a bubbling bed reactor containing a Pd-Ni-Ag-M / Al2O3 catalyst, and then 2-butyne is converted into butane. The method has the advantages that the processes are simple, no wastewater is drained, the denitrification precision is high, no material is lost, and polymerization side reactions can be effectively inhibited.

The invention discloses a high-purity piperylene preparation method, wherein isoprene and cyclopentadiene are removed from C5 distillate, the obtained C5 distillate is used as a raw material, and treatment is performed through adsorption and extraction rectification to obtain the high-purity piperylene. With the method of the present invention, a small of difficultly-removed cyclopentadiene and 2-butyne can be effectively removed from piperylene; the process is simple and effective; and with the method, the high-purity piperylene with the cyclopentadiene content of less than 50 ppm and the 2-butyne content of less than 20 ppm can be obtained.

The invention discloses an environment-friendly high-brightness medium-phosphorus chemical nickel-plating additive which is composed of components A and B, wherein the component A comprises the following raw materials: a 2-5mg / L mixture of nano copper and a soluble copper salt, 2-4mg / L rhenium sulfate, 1-4mg / L sodium allysulfonate (ALS), a complexing agent, a stabilizer, and 20-40g / L NaOH; the component B comprises the following raw materials: 1-4mg / L 1,4-bis(2-hydroxyethoxy)-2-butyne (BEO), 1-3mg / L N,N-diethylaminopropyne (DEP), 1-4mg / L dibenzenesulfonimide (BBI), and 2-4mg / L sodium hydroxymethanesulphonate (PN). The formula of the environment-friendly high-brightness medium-phosphorus chemical nickel-plating additive provided by the invention contains no heavy metal ions such as cadmium and lead, and is harmless to the environment; if applied to a chemical nickel-plating solution, the additive is capable of keeping the plating solution stable so that the obtained coating is even and compact, low in porosity, high in brightness and good in nitric acid resistance; more specifically, even though the nickel coating is soaked in concentrated nitric acid for 300 seconds, the nickel coating does not change color.

The invention belongs to the field of pharmaceutical chemicals, and in particular relates to a preparation method of linagliptin and an intermediate thereof. The preparation method comprises the following steps: carrying out Mitsunobu reaction on a compound I and 2-butyne-1-alcohol in an organic solvent in the presence of trialkyl phosphine and an azo-reagent to obtain a linagliptin intermediate compound II; carrying out substitution reaction on the compound II and (R)-3-aminopiperdine by taking isopropanol as a solvent and tri-n-butylamine as an acid-binding agent to obtain a compound III; and carrying out alkylation reaction on the compound III and 4-methyl-2-chloro-methyl-quinazolin to obtain linagliptin. According to the preparation method provided by the invention, the Mitsunobu reaction is innovatively adopted to prepare the compound II, so that the preparation method has the advantages of mild reaction condition, reasonable operation, high selectivity, high product quality and the like. Moreover, by controlling the reaction condition, the compound III and R-3-aminopiperdine or an inorganic acid salt or an organic acid salt thereof are directly subjected to nucleophilic substitution to generate linagliptin, and the method does not have protection and de-protection processes of amino groups, so that the reaction steps are reduced, the reaction process is simpler, the cost is reduced, and the purity of an obtained product is relatively improved.

The invention provides a manufacturing method of a nickel-tungsten plating layer. A plating solution consists of 0.15-0.45 mol / L nickel chloride, 0.1-0.25 mol / L nickel sulfate, 0.1-0.2 mol / L sodium sulfate, 0.1-0.3 mol / L sodium hydrogen phosphate, 0.5-2 mol / L citric acid, 0.001-0.005 ml / L OP-10, 0.1-0.2 g / L 1,4-dihydroxy-2-butyne, and 0.1-0.4 mol / L sodium tungstate. An electrodeposition technology comprises the following steps of enabling the current density to be 3-15 A.dm<-2>, and enabling the temperature of the plating solution to be 20-40 DEG C. The manufacturing method disclosed by the invention has the advantages of being simple in technology, low in cost, simple in pre-processing, high in stability of the plating solution, long in cycle life and the like, so that large-scale production of the nickel-tungsten plating layer can be realized.

The invention provides a preparation method of a linagliptin intermediate for treating type-II diabetes mellitus. According to the preparation method of the intermediate 8-bromo-3,7-dihydro-3-methyl-9-(2-butynyl)-1H-purine-2,6-dione, 8-bromo-3,7-dihydro-3-methyl-1H-purine-2,6-dione reacts with 2-butyne in an organic solvent in the presence of a copper catalyst and a cocatalyst to prepare the 8-bromo-3,7-dihydro-3-methyl-9-(2-butynyl)-1H-purine-2,6-dione. Operation is simple, conditions are mild, relatively high yield and purity are obtained, and the preparation method is suitable for large-scale industrial production.

A method for separating a petroleum cracking C5 fraction through an acetonitrile process comprises the following steps: removing most of 2-butyne and 2-methyl-1-butenyl-3-alkyne from the petroleum cracking C5 fraction in advance; adopting a continuous thermal dimerization-rectification-thermal dimerization-rectification process to make a reaction be carried out toward a dicyclopentadiene generation direction, and carrying out a series of separation processes to obtain highly pure polymeric isoprene; and carrying out flash evaporation on water washed acetonitrile, returning the evaporated acetonitrile to a double extraction desorption tower, pumping off parts of a circulating solvent, purifying, and removing polymers in the solvent. The method has the following advantages: the solvent keeps high selectivity; production of an m-pentadiene product with the purity being greater than 70% and an m-pentadiene product with the purity being greater than 95% is realized by adopting same flow according to different uses, and cyclopentene with the purity being greater than 99.5% and cyclopentane with the purity being greater than 99.8% can also be obtained; and long-term stable running of a C5 separation device is guaranteed.

The invention relates to a preparation method and application of 1,4-diboric acid ester-2-butyne. The preparation method comprises the steps of performing pinacol ester reaction of trichloro ethylene and iodine methylene boric acid by regarding n-butyllithium as alkali, and obtaining a product 1,4-diboric acid ester-2-butyne through separation and purification; performing tandem propargyl / guildline alkenyl reaction on 1,4-diboric acid ester-2-butyne and aromatic aldehyde to prepare a 1,3-butadiene-2,3-di-secondary alcohol compound. The preparation method is simple and convenient to operate; the used reagents are nontoxic, green and environment-friendly; the prepared 1,3-butadiene-2,3-di-secondary alcohol compound can be further subjected to derivatization through Diels-Alder or Shapless epoxidation reaction, and is an important organic synthon.