110 results about "Sodium tert-butoxide" patented technology

The invention discloses a solid basic catalyst, a preparation method of the solid basic catalyst and an application of the solid basic catalyst in ester exchange reaction. The solid basic catalyst catalyzes the ester exchange reaction by the reaction of metal organic compound and hydroxyl on a carrier under the moderate conditions to synthesize dimethyl carbonate. The solid basic catalyst provided by the invention consists of metal organic alkali and the carrier. The metal organic alkali is linked to the carrier in bond-forming manner; the metal organic alkali is one or more of lithium methoxide, lithium ethoxide, lithium isopropoxide, lithium n-butoxide, lithium tert-butoxide, sodium methoxide, sodium ethoxide, sodium isopropoxide, sodium n-butoxide, sodium tert-butoxide, potassium methoxide, potassium ethoxide, potassium isopropoxide, potassium n-butoxide and potassium tert-butoxide; the carrier is one or more of silicon oxide, aluminium oxide, titanium oxide, zirconia, mesoporous silicon oxide synthesized by the template method, mesoporous aluminium oxide synthesized by the template method, mesoporous titanium oxide synthesized by the template method, and mesoporous zirconia synthesized by the template method.

The invention relates to a synthetic method of cholesterol. The synthetic method of the cholesterol specifically comprises the following steps that 1, firstly, triphenylphosphine and 1-chlorine-4-methylpentane are used to react to obtain a 4-methyl pentyl triphenyl phosphonium chloride solution, then potassium tert-butoxide or sodium tert-butoxide is added to react to obtain a witting reagent, a witting reaction occurs by adding pregnenolone into the witting regent, and a compound 03 is obtained through extracting after complete reaction; 2, under the action of chirality phosphine ligand and a rhodium catalyst, an asymmetric hydrogenation reaction occurs to the compound to obtain the cholesterol. According to the synthetic method of the cholesterol, a 6-step reaction of an existing method is simplified into a 2-step reaction, and meanwhile the ring-opening reaction consuming a large amount of hydrochloric acid and zinc powder is omitted. The technology is simple, the consumption of raw materials is less, the yield is high, the cost is low, environmental protection is achieved, so that the economical effect and the environmental protection are achieved, and the industrial implementation is facilitated.

The invention relates to an efficient cyhalothrin and a manufacturing technology thereof, the manufacturing technology is as follows: (1) layer addition-reaction materials are 3, 3-dimethyl-4-pentenoic acid methyl ester and trichlorotrifluoroethane; (2) cyclization- reaction materials are tertiary butyl alcohol, Bifenthrin and sodium tert-butoxide; (3) elimination of hydrolysis-reaction materials are potassium hydroxide and cyclic Bifenthrin, and by exsolution, hydrolysis, separation and filtration 2-cis-3-(2-chloro-3, 3, 3-trifluro-1-propenyl)-2, 2-dimethyl cyclopropane carboxylic acid can be prepared; (4) chloroformylation-reaction materials are thionyl chloride, methylbenzene and 2-cis-3-(2-chloro-3, 3, 3-trifluro-1-propenyl)-2, 2-dimethyl cyclopropane carboxylic acid, and by exsolution and distillation, 3-(2-chloro-3, 3, 3-trifluoro-1-propenyl)-2, 2-dimethylcyclopropane carbonyl chloride is obtained; (5) esterification- reaction materials are phenylate aldehyde, sodium cyanide, PTC and 3-(2-chloro-3, 3, 3-trifluoro-1-propenyl)-2, 2-dimethylcyclopropane carbonyl chloride, by water rinse, exsolution and distillation, the cyhalothrin is prepared; and (7) epimerization-inoculating crystal is added for carrying out an epimerization reaction, and after the reaction, an end product-the efficient cyhalothrin is obtained by filtration and drying. As the invention adopts the technical proposal, the efficient cyhalothrin prepared by the invention greatly shortens the technological route and obviously improves the reaction efficiency through the improvement of technical skills, thereby reducing the cost of industrialization.

The invention discloses a preparation method of selexipag, and relates to the technical field of preparation of drugs for treating pulmonary hypertension. The preparation method comprises the following steps: adding a compound as shown in the formula I and a compound as shown in the formula II in an organic solvent; adding alkali; stirring at the reaction temperature of 10-40 DEG C and carrying out Williamson reaction; synthesizing a compound as shown in the formula A, namely the selexipag. The organic solvent is 1-4-dioxane; the alkali is sodium tert-butoxide, potassium tert-butoxide or mixed alkalis of sodium tert-butoxide and potassium tert-butoxide. A synthetic route is reasonable in design, reaction conditions are mild, the cost is low, special equipment is not required, a product is high in purity and high in yield, and aftertreatment is simple and convenient, so that the preparation method of the selexipag is suitable for industrial production.

The invention relates to a preparation method of di-tert-butyl dicarbonate and belongs to the technical field of synthesis of pharmaceutical intermediates. The preparation method comprises the following steps: adding metal sodium into xylol; heating to obtain sodium sand; then dropwise adding tert-butyl alcohol and carrying out pumping filtration to obtain sodium tert-butoxide; dissolving the sodium tert-butoxide into petroleum ether; introducing carbon dioxide and reacting to obtain a monoester sodium salt solution; adding a catalyst and slowly dropwise adding diphosgene to react; after reacting, standing and carrying out the pumping filtration; and washing with water, drying, distilling, cooling and crystallizing to obtain the di-tert-butyl dicarbonate. According to the preparation method, the sodium tert-butoxide is prepared from the metal sodium and the di-tert-butyl dicarbonate is prepared from the sodium tert-butoxide; a pumping filtration method is used for replacing a previous distillation method, so that the process is simpler and more energy is saved; the petroleum ether is used for replacing n-hexane and toluene, so that the production cost is reduced and a product is easier to purify; and finally, after the reaction, the pumping filtration is carried out and then water washing is carried out, so that the amount of wastewater is reduced and the environment-friendly treatment cost is reduced.

The invention discloses a photoelectric material and a preparation method thereof and application to an organic electronic device. The preparation method of the photoelectric material includes the steps that a halogenated compound of M1 or M2 is prepared firstly, wherein M1 or M2 monomers serve as raw materials, N-bromosuccinimide or liquid bromine is added, in an organic solvent of concentrated sulfuric acid or hydrogen peroxide, a reaction is conducted under a normal-temperature or heating and stirring conditions, purification is conducted, and the halogenated compound of M1 or M2 is obtained; then secondary amine is prepared through a C-N coupled reaction, wherein Pd2(dba)3 and DPPF are firstly added to a container, after stirring in a benzene series solvent, the halogenated compound of M1 or M2 is added, primary amine of Ar1 or Ar4 and sodium tert-butoxide are added, and heating reflux is conducted; finally the photoelectric material is prepared. A D-A-D-A type non-conjugate polymer is synthesized through a C-N coupling polymerization method, in addition, a side chain with an electron-donating group is arranged, LUMO and HOMO electron clouds are slightly overlapped, and therefore the characteristic of thermotropic delayed fluorescence can be easily achieved.

The invention relates to a synthesis method of polyuralcohol, belonging to polymer technical field, which comprises that adds dihalide aromatic ketone, sodium tert-butoxide NaOt-Bu, 1, 1'-dinaphthalene-2, 2'-diphenylphosphino BINAP, aromatic diamine and Pd2(dba)3 into a three-mouth flask with nitrogen gas feeding in turn, wherein the mole ratio is 1:1:2.8:0.03:0.01, adds N, N-dimethylacetamide until the monomer density is 0.5-0.65mol / L, increases temperature from 20DEG C to 100DEG C, keeps for 4-6h, increases temperature from 100DEG C to 150-200DEG C, keeps for 20-24h, cools to 20DEG C, adds the mixture of ammonia and methanol at the ratio of 1:4(L / L), mixes, stands for 1h, washes via the mixture of ammonia and methanol for three times, filters, dries at vacuum for 6h, mixes and dissolves poly(imino ketone) and benzoyl chloride in tetrahydrofuran for 2-12h at 1-3DEG C, to obtain polyuralcohol to be dried. The synthesized polyuralcohol Tg is higher than 190DEG C and TD is higher than 450DEG C, with better heat stability and dynamic mechanical stability.

The invention discloses a method for synthesizing 1, 2, 3-triazole by cycloaddition reaction of base catalysis enaminone and azide. According to the method, propargyl esters, primary amine and sulfonyl azide serve as raw materials, the enaminone with an NH structure is generated in situ, the raw materials are stirred at room temperature for two hours under catalysis of secondary amine and sodium tert-butoxide, 1, 4-bis-substituted-1, 2, 3-triazole compounds can be obtained with high yield, and products are subjected to chromatographic purification by a silica gel column. The method has the advantages that reaction conditions are mild, reaction can be smoothly realized at the room temperature, reaction time is short, two steps can be finished totally for four hours, the raw materials are green and low in cost, ferric chloride used in first-step operation is an environment-friendly catalyst, metal is omitted in second-step reaction, the method is greener than most methods for synthesizing similar compounds, and the method is simple in overall operation and suitable for large-scale production.

The invention discloses a method for preparing a compound 2-(imidazo [1,2-a] pyridine-3-yl) acetonitrile, which is a new method for preparing a key intermediate of minodronic acid, comprising the steps of: with a compound 3- imidazo [1, 2-a] pyridine carboxaldehyde with the formula (II) and a compound tosylmethyl isocyanide with the formula (III) as raw materials, carrying out chemical reaction in an organic solvent containing glycol dimethyl ether and an alkaline medium of potassium tert-butoxide or sodium tert-butoxide; separating and purifying to obtain the compound 2-(imidazo [1, 2-a] pyridine-3-base) acetonitrile, wherein the process of the chemical reaction is disclosed in the specification of the invention. In the invention, by means of the method for preparing the compound with the formula (I), the reaction procedure is shortened, the technical process of the whole reaction is simplified, the use of a highly toxic material sodium cyanide is avoided, the operability of the reaction is strong, the yield is high, and the obtained product has high purity, lower cost, and is easy for the application in the industrialized production.

The invention discloses an anthracene nitrogen-containing organic light-emitting compound and a preparation method and application thereof, the specific structure of the anthracene nitrogen-containingorganic light-emitting compound is as shown in the general formula 1 in the specification, and the preparation method comprises the following steps: taking methylbenzene as a solvent; reacting the raw material A with the raw material B in the presence of sodium tert-butoxide, tris (dibenzylideneacetone) dipalladium and tris(tert-butyl)phosphorus to obtain an intermediate product C, reacting the intermediate product C with NBS by taking dichloromethane as a solvent to obtain an intermediate product D, and reacting the intermediate product D with a mixed solution of methylbenzene, ethanol and water by taking a mixed solution of methylbenzene, ethanol and water as a solvent; and reacting the intermediate product D with a raw material E in the presence of potassium carbonate and tetrakis(triphenylphosphine)palladium to finally obtain the compound shown in the general formula I. The anthracene derivative provided by the invention has relatively high electron transmission performance, and can improve the electron transmission efficiency of a device and can prolong the service life of the device when being applied to an organic electroluminescent device. In addition, the preparation method provided by the invention is simple, easy to operate and suitable for industrial popularization.

The invention discloses sodium tert-butoxide and a preparation method thereof. The preparation method comprises the following steps: (1) taking methylbenzene or heptanes as a reaction medium, adding sodium amide and tertiary butanol, mixing and stirring to dissolve to obtain a mixed solution; (2) heating the mixed solution to 70-110 DEG C for reaction to obtain a crude product of sodium tert-butoxide till the reaction is completed; (3) rectifying the crude product of the sodium tert-butoxide to obtain a finished product of the sodium tert-butoxide. The preparation method disclosed by the invention has relaxed reaction conditions, is small in danger in the production process, simple in aftertreatment process of products and short in drying time, and the product yield is up to 99% or above.