72 results about "Tert-Butyl chloride" patented technology

The invention is a manufacturing method of diamante amine hydrochlorate. The invention adopts 1, 3-dimethyl adamantine to reacts with tert-butylchlorine and gets 1-chlorine-3, 5-dimethyl adamantine; then reacts with acetamide directly, the educt from water reacts with sodium hydroxide in ethanediol or glycerine solvent, extracts by acetic ester, condenses, and blow in dry hydrochloride gas and gets the coarse product. There gets the pure product through alcohol-acetic ester recrystallization.

The invention discloses a novel technology for preparing a bactericide tebuconazole through a solvent-free method. The technology comprises the steps that 2-tertiary butyl-2-(4-chlorphenyl ethyl)ethylene oxide and 1,2,4-triazole are taken as raw materials and react under the catalytic action of an alkaline catalyst and a phase transfer catalyst, and aftertreatment is conduced on a reaction product to obtain the product tebuconazole. According to the technology, no solvent is used in the synthesizing reaction process, and therefore the solvent cost input is reduced; in addition, due to the fact that the reaction concentration is high, the reaction speed is greatly increased, the product yield is significantly increased, a separation method is easy and convenient to operate, and industrialized production is easy.

The invention relates to a method for preparing 3,3-dimethyl butyraldehyde. The method comprises the following steps: (1) vacuumizing a closed reaction kettle, adding a dichloromethane solvent, dripping vinyl acetate, introducing a catalyst after dripping is ended, and introducing hydrogen chloride gas, so that the pressure reaches 0-1MPa, slowly dripping tert butyl chloride for reacting, removing excessive hydrogen chloride gas after the reaction is ended to obtain a distillation product, raising the temperature and distilling to obtain 1-chloro-3,3-dimethyl butyl acetate; and (2) adding the 1-chloro-3,3-dimethyl butyl acetate and water into the reaction kettle, controlling the temperature to be 120 DEG C, performing hydrolysis disproportionation on the 1-chloro-3,3-dimethyl butyl acetate to obtain a hydrolysis disproportionation reaction mixture containing 3,3-dimethyl butyraldehyde, and distilling and purifying to obtain the 3,3-dimethyl butyraldehyde. According to the method disclosed by the invention, the production cost is low, the production process is shortened, the reaction conditions are mild, the production safety is high, and the preparation method is simple in preparation process, easy to control, high in yield and safe.

The present invention relates to a preparation method of alkyl benzene solvent. It is made up by adopting tert-butyl chloride or tert.-butyl alcohol and dimethylbenzene or ethylbenzene through a certain reaction process. Its reaction temperature is 0-50 deg.C, reaction pressure is normal pressure, the mole ratio of tert.-butyl chloride or tert.-butyl alcohol and dimethylbenzene or ethylbenzene is 1.5-1-1:1.5, the catalyst dose is 0.5-20% of solvent weight. The catalyst is an ion liquid catalyst or one of anhydrous aluminium trichloride, anhydrous iron trichloride, sulfuric acid and hydrofluoric acid. The invented alkyl benzene solvent purity is 98%-100%, boiling range is 200-215 deg.C and relative density is 0.86-0.88. It can be used for synthesis of phthalocyanine copper.

This invention discloses a synthesis method for Neotame. The said method includes the following steps: (1) carrying out a reaction of tert-butanol with hydrochloric acid to obtain tert-butyl chloride; (2) adding catalyst in tert-butyl chloride, and charging ethylene gas and reacting to obtain 3, 3-dimethyl-1-chlorobutane; (3) oxidating 3, 3-dimethyl-1-chlorobutane to obtain 3, 3-dimethyl butyraldehyde, and purifying; and (4) carrying out a reaction of 3, 3-dimethyl butyraldehyde with aspartame to form imine, and catalytic-hydrogenating to obtain Neotame. The invention has the advantages of simple process, easy operation, low cost, and high purity of the product.

The invention belongs to the technical field of compound preparation and discloses a chemical synthetic method for preparing p-tert-butylbenzylamine. The chemical synthetic method is characterized by comprising the following steps: firstly, reacting p-tert-butylbenz with urotropine to prepare quaternary ammonium salt, carrying out prehydrolysis on the quaternary ammonium salt by hydrochloric acid and alcohol solution, filtering, evaporating a solvent to obtain p-tert-butylbenzylamine hydrochloride solid; using the p-tert-butylbenzylamine hydrochloride solid as a raw material, using hydrochloric acid and water to carry out secondary hydrolysis on the p-tert-butylbenzylamine hydrochloride solid, reducing pressure, evaporating the solution to be dried, obtaining faint yellow solid matter, and using 40 percent sodium hydroxide solution to adjust pH of the faint yellow solid matter to be 8 to 12, thus obtaining the p-tert-butylbenzylamine. The chemical synthetic method can effectively remove a large amount of impurities in the p-tert-butylbenzylamine prepared by the existing method and obtain the p-tert-butylbenzylamine with high purity.

The invention relates to a preparation method of industrial musk tonalide, which comprises the following steps: carrying out Friedel-Crafts alkylation by using p-isopropyl toluene and 2,3-dimethyl-1-butene as raw materials and using tertiary butyl chloride as a hydrogen absorption agent to synthesize an intermediate 1,1,3,4,4,6-hexamethyl tetrahydronaphthalene; and in a dichloromethane solvent, carrying out Friedel-Crafts alkylation on the intermediate used as the raw material and acetyl chloride, thereby obtaining the product musk tonalide (7-acetyl-1,1,3,4,4,6-hexamethyl tetrahydronaphthalene, AHMT). Compared with the existing method and technology, the method provided by the invention is simple to operate, has the characteristics of high reaction speed, high yield and the like, and realizes industrial production; and the product can be simply purified by thermally dissolving out pigments by using anhydrous alcohol without distillation or rectification.

The invention discloses a method for synthesizing 1-cyclopropyl-naphthyl by virtue of 1-vinyl-naphthyl and belongs to the technical field of organic synthesis. The method comprises the steps of under nitrogen protection and the condition of and ice bath, slowly dripping 1-vinylnaphthalene into tert-butylmagnesium chloride as a Grignard reagent with the concentration of 3M, wherein the molar ratio of the 1-vinylnaphthalene to the tert-butylmagnesium chloride is 1:(0.3-2); after dripping, adding 1-6mol methylenehalide and 0.3-2mol tert-butylmagnesium chloride as the Grignard reagent with the concentration of 3M, after reacting for 1-6 hours, quenching the reaction by virtue of a saturated ammonium chloride solution, extracting by virtue of ethyl acetate, evaporating the ethyl acetate by virtue of decompression, and carrying out recrystallization by virtue of methylbenzene to obtain a product. With the adoption of the method, with the 1-vinylnaphthalene and the methylenehalide as cheap chemical products as initial raw materials, the 1-cyclopropyl-naphthyl is synthesized by virtue of a one-step method; as the reaction conditions are mild and the operation is convenient, the method is suitable for industrial large scale production, and the synthesis cost of the 1-cyclopropyl-naphthyl is greatly lowered.

The invention relates to a method for synthesizing 3-(tert-butyl)phenol. The method includes the following steps that 4-tert-butyl-1-chlorobenzene serves as a raw material and is nitrated to obtain 1-chlorine-4-tert-butyl-2-nitrobenzene; the 1-chlorine-4-tert-butyl-2-nitrobenzene is reduced to generate 3-tert-butylaniline; the 3-tert-butylaniline is diazotized and subjected to a hydrolysis reaction, and the 3-(tert-butyl)phenol is obtained. According to the path, the raw material is cheap and easy to get, elementary reaction conditions of the steps are mild, after-treatment is simple, the four-step reaction total yield is high, the 3-(tert-butyl)phenol with the purity higher than 97% can be obtained through distilling, and industrial production prospects are achieved.

The invention discloses a method for preparing 5-tert butyl meta-xylene by adopting a tubular reactor. The method comprises the following steps: S1, preparing an auxiliary catalyst; S2, mixing the auxiliary catalyst with aluminum trichloride, thus preparing a compound catalyst; mixing the compound catalyst with meta-xylene, thus obtaining a raw material A; using tert-butyl chloride as a raw material B, and feeding the raw material A and the raw material B for reacting by respectively adopting two feeding modes; S3, carrying out aftertreatment on a reaction solution after completing reaction, thus obtaining a 5-tert butyl meta-xylene finished product. According to the method disclosed by the invention, the reaction time is greatly shortened, the conversion rate is remarkably increased, generation of byproducts is reduced, the method has the advantages that operation is simple and clear and is safe and reliable, the yield of the prepared 5-tert butyl meta-xylene is up to 95 percent or above and is increased by 20 percent or above than the yield of a traditional technology, and the problems that during a stirring process of a traditional tank reactor, influence of backmixing appears,and charging and discharging are difficult are solved.

The invention discloses a preparation method of bis(ditert-butyl phenyl phosphine)palladium dichloride. The preparation method includes the following steps that (1) palladium sponge is dissolved in royal water, concentrated, saltpetre-removed and then filtered, and a filtrate is diluted with water to obtain a solution of palladium chloride acid; and then the filtrate is dropwise added into an ethanol solution of 1,5-cyclooctadiene, reacted until precipitation is no longer precipitated, and filtration is conducted to obtain 1,5-cyclooctadiene palladium chloride; (2) a phenyl grignard reagent isdropwise added into a tetrahydrofuran solution of bi tertiary butyl phosphorus dichloride to obtain a tetrahydrofuran solution of bis(ditert-butyl phenyl phosphine); (3) the tetrahydrofuran solutionof the bis(ditert-butyl phenyl phosphine) is dropwise added into a tetrahydrofuran solution of the1,5-cyclooctadiene palladium chloride; (4) filtration is conducted, and a filter cake is washed with anhydrous ethanol; and (5) drying is conducted. According to the preparation method, the 1,5-cyclooctadiene palladium chloride prepared by taking the palladium chloride acid as a metal source is used as a reaction precursor, the prepared bis(ditert-butyl phenyl phosphine) is used as an ligand, the ligand does not require purification, and the yield of products is high.

The invention discloses a preparation method for bis[di-tert-butyl(4-dimethylaminophenyl)phosphine]dichloropalladium. The preparation method comprises the following steps that 1, a Grignard reagent isprepared from the raw materials of N, N-dimethyl p-haloaniline and magnesium chips; 2, the Grignard reagent is taken and cooled, then a catalyst is added for reaction, then di-tert-butylchlorophosphane is dropwise added, and heating is carried out for reaction so as to obtain di-tert-butyl-4-dimethylaminophenylphosphine; 3, the di-tert-butyl-4-dimethylaminophenylphosphine is purified; and 4, complexing bis(acetonitrile)dichloropalladium and the purified di-tert-butyl-4-dimethylaminophenylphosphine so as to obtain a target product. The preparation method has the advantages that the di-tert-butyl-4-dimethylaminophenylphosphine is purified, the high-purity di-tert-butyl-4-dimethylaminophenylphosphine is used for reacting with the bis(acetonitrile)dichloropalladium, and therefore the yield loss of the noble metal palladium is greatly reduced, the preparation cost is greatly lowered, and the method has a good practical value.

The present invention provides an optical polyimide precursor for use in making a polyimide. The precursor is defined by the following formula:

wherein X is Cl, Br, oxo-halide, or fully halogenated alkyl, and A is a divalent aromatic or halogenated aromatic moiety. The present invention provides a method of preparing a diamine compound for use as an optical polyimide precursor. The method includes the steps of dissolving 2-chloro-5-nitrobenzotrifluoride and a diol in N,N-dimethylacetamide to form a solution, adding potassium carbonate, tert-butylammonium chloride and copper powder to said solution and heating the resulting mixture, removing the copper, precipitating and recrystallizing a dinitro-compound resulting from heating the mixture, and dissolving the dinitro-compound and reducing the dinitro-compound to yield a diamine compound.

A method for the synthesis of 1,3-di(chloropropyl)-5-tert-butyl benzene includes the steps of conducting Friedl-Crafts alkylation of 1,3-diisopropyl benzene by tert-butyl chloride in the presence of an alkylation catalyst to obtain 1-tert-butyl-3,5-diisopropylbenzene; peroxidizing the 1-tert-butyl-3,5-diisopropyl benzene by gaseous oxygen in the presence of a peroxidation catalyst in a basic solution to obtain 1,3-di(peroxypropyl)-5-tert-butylbenzene; reducing the 1,3-di(peroxypropyl)-5-tert-butylbenzene with a reducing agent to 1,3-di(hydroxyl propyl)-5-tert-butylbenzene; and chlorinating the 1,3-di(hydroxypropyl)-5-tert-butylbenzene to obtain 1,3-di(chloropropyl)-5-tert-butyl benzene.

The invention provides a preparation method of a tonalide intermediate HMT. The preparation method comprises the steps of mixing p-cymene, sulfuric acid, phosphoric acid and aluminum trichloride in acertain ratio in a reactor; then mixing and dripping 2,3-dimethyl-1-butene and tert-butyl chloride into the reactor, and reacting at a room temperature for 1 hour to generate the tonalide intermediateHMT, wherein the molar ratio of 2,3-dimethyl-1-butene to tert-butyl chloride to p-cymene to aluminum trichloride to sulfuric acid to phosphoric acid to dichloroethane to cyclohexane is 0.5-1.5 to 0.9-1.3) to 1.4-2.6 to 0.07-0.13 to 0.006-0.013 to 0.006-0.012 to 0.7-1.5 to 0.6-1.4; and directly transferring the reacted substances to a rectification column for rectification and purification to obtain a tonalide intermediate HMT product. The HMT product with higher yield can be obtained from new reaction substances, the purification method is improved, and the conventional recrystallization purification method is changed to reduce pollution and lower the production cost.

The invention relates to a method for preparing a bis(4-tert-butyl benzyl)sulfide product, belonging to the technical field of preparation of medical intermediate compounds and polymer antioxidants. The method comprises the following step: in the presence of both an emulsifier and a phase-transfer catalyst, reacting 4-tert-butyl benzyl chloride and a sodium sulfide water solution used as raw materials in an organic solvent-water system, wherein the proportioning of the raw materials is as follows: the mol ratio of the 4-tert-butyl benzyl chloride to the sodium sulfide is 1:(0.5-0.9); the mass ratio of the 4-tert-butyl benzyl chloride to the organic solvent is 1:(0.8-1.6); the mass ratio of the 4-tert-butyl benzyl chloride to the emulsifier is 1:(0.008-0.033); the mass ratio of the 4-tert-butyl benzyl chloride to the phase-transfer catalyst is 1:(0.008-0.033); the reaction temperature in the reaction process is 50-70 DEG C; and the reaction time is 150-240 minutes. Thus, high raw material conversion rate and product yield are achieved.

The invention relates to a method for preparing tert-butyldimethyl chlorosilane, which is characterized by comprising the following steps of: a, in a synthesis kettle, putting 10 to 15 weight parts of magnesium into 160 to 240 volume parts of mixed solvent consisting of ether and cyclohexane, dripping mixed solution consisting of 35 to 55 weight parts of tertiary butyl chloride and 50 to 78 weight parts of dimethyl dichlorosilane into the mixed solvent at the temperature of between 40 and 55 DEG C, a preserving heat for 2.5 to 3.5 hours after the dripping is finished to obtain a synthesized material; b, transferring the synthesized material to a dissolution kettle, cooling the synthesized material to between 10 and 15 DEG C, then dripping 400 to 600 volume parts of 25 to 30 percent hydrochloric acid into the dissolution kettle, standing and demixing the solution, and removing wastewater at the bottom to obtain upper liquor; and c, transferring the upper liquor in the dissolution kettle to a rectification kettle to perform purification, and removing the solvent to obtain a tert-butyldimethyl chlorosilane product. The method has the advantages of simple synthesis process, high safety and stable product yield.

The invention relates to the field of medicine, in particular to a method for catalyzing synthesis of an atazanavir intermediate by a carbonyl reductase CLEAs. The method uses (S)-tert-butyl (4-chloro-3-carbonyl-1-phenylbutyl-2-yl) carbamate as a substrate and a carbonyl reductase NaSDR crosslinked aggregate as a catalyst, and the catalyzing synthesis of tert-butyl ((2S, 3R)-4-chloro-3-hydroxy-1-phenylbutyl-2-yl)) carbamate is carried out in a system in which a co-substrate, a co-solvent and a buffer solution are present. By the adoption of the method for the catalyzing synthesis of the atazanavir intermediate by the carbonyl reductase CLEAs, a reaction system is simpler, additional expensive coenzymes are not necessary, and glucose is not required to participate in a coenzyme cycle; in addition, the reaction temperature is closer to room temperature; the carbonyl reductase NaSDR crosslinked aggregate as a biocatalyst has better temperature stability and pH stability and can be reusedin 6 batches, so that the method is more energy-saving and environmentally friendly, and cost is further reduced.

The invention discloses a method for synthesizing 4-tert-butyl benzyl chloride. The method comprises the following steps of: (1) weighing a certain amount of tertiary butyl, formaldehyde, hydrochloric acid and formic acid, and mixing the raw materials with stirring; (2) heating the mixed raw materials in water bath to 60 to 70 DEG C, controlling the reaction temperature to be 70 to 75 DGE C and reacting for 10 and 20 hours; (3), cooling to room temperature, separating out rough products, washing with water, 8 weight percent K2CO3, water and diethyl ether in turn, and adding anhydrous calcium carbonate for drying; and (4) distilling under normal pressure and then distilling under reduced pressure to obtain the 4-tert-butyl benzyl chloride. In the method, the conversion rate of reaction is high and is about 50 to 60 percent, yield is kept in a high level and is more than 70 percent, the operation process is simple, and the method is environmental-friendly, and has obvious economic benefit, social benefit and market competitiveness.