165 results about "Tert-Butyl formate" patented technology

The invention provides a method for preparing baricitinib. The method comprises the following steps: by taking 4-pyrazol boric acid pinacol ester (10) as an initial raw material, performing Michael addition reaction on the initial raw material and 3-(icyanomethylene) azacyclo-cyclobutane-1-tert-butyl formate (11) so as to prepare an intermediate 12, and performing catalytic coupling reaction on 12 and 13, thereby preparing an intermediate 14; removing two-molecule tert-butyl formate of the intermediate 14, thereby preparing an intermediate 15; performing sulfamide reaction on the intermediate 15 and ethanesulfonyl chloride in an organic solvent, thereby obtaining a final product baricitinib (1). The method for preparing baricitinib has the advantages that the raw materials are easy to obtain, the process is simple, the operation is convenient, the reaction yield is high when being compared with that of document records, the atom utilization rate is high, industrial production can be easily achieved, and the like. The reaction general formula is as shown in the specification.

The invention discloses a magnetic slot wedge and a production method thereof. The magnetic slot wedge comprises 18 percent to 20 percent of 943 unsaturated polyester resins, 0.5 percent to 1 percent of an internal releasing agent, 0.2 percent to 0.5 percent of tert-butyl peroxy benzoate, 0.1 percent to 0.3 percent of benzoyl peroxide, 54 percent to 57 percent of magneto-increasing material and 24 percent to 25 percent of alkali free glass fiber. The production method comprises the steps that: 1. the unsaturated polyester resins, the internal releasing agent and a peroxide evocating agent are prepared into an adhesive according to proportion; 2. a mould is heated to be 150 DEGC -200 DEG C and extraction speed is 0.8-1.40r / min; 3. the alkali free glass fiber soaking the adhesive is treated with pultrusion by the mould; 4. cooling and cutting are carried out; 5. the cut slot wedge is treated with head grinding; 6. the surface of the slot wedge is treated with paint treatment to become bright and clean with no burr; and 7. airing, detecting and packaging are carried out. The magnetic slot wedge has high magnetoconductivity, high cleavage strength, great bending strength and simple production method.

The invention discloses a preparation method of baricitinib. The method comprises the following steps: performing a substitution reaction on 4-chloro-7H-pyrrolo[2,3-d]pyrimidine (II) serving as a raw material and benzene sulfonyl chloride in the presence of an alkali to obtain an intermediate III; then, performing a Suzuki coupling reaction on the intermediate III and 4-pyrazole-4-boronic acid pinacol ester in the presence of a palladium catalytic system and an alkali to obtain an intermediate V; then performing a Michael addition reaction on the intermediate V and 3-(cyanomethylene)azetidine-1-tert-butyl formate in the presence of a catalyst to obtain an intermediate VII; then removing Boc protection from the intermediate VII under the action of hydrochloric acid to obtain an intermediate VIII; then performing a sulfoamidate reaction on the intermediate VIII and ethyl sulfonyl chloride in an organic solvent in the presence of an alkali to obtain an intermediate IX; lastly, removing benzenesulfonyl protection from the intermediate IX under the action of tetramethylammonium fluoride or tetrabutylammonium fluoride or a trihydrate of the tetramethylammonium fluoride or the tetrabutylammonium fluoride to obtain baricitinib (I). Compared with the prior art, the method has the advantages of adoption of readily-available raw materials, low cost, high product yield and easiness for industrial production.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of 7-bromopyrrolo [2, 1-f][1, 2, 4] thiazine-4-amine, which comprises the followingsteps: 1) synthesizing an intermediate I, namely 1-Boc-1-aminopyrrole, by taking tert-Butyl carbazate and 2, 5-dimethoxytetrahydrofuran as raw materials; 2) enabling the intermediate I to react withan isocyanate methanesulfonate to synthesize an intermediate II, namely 1-Boc-1-amino-(9ci)-1H-pyrrole-2-carbonitrile; 3) performing deamination protection on the intermediate II under an acidic condition to obtain an intermediate III, namely 1-amino-(9ci)-1H-pyrrole-2-carbonitrile hydrochloride; 4) performing a ring closing reaction on the intermediate III and formamidine acetate to obtain an intermediate IV, namely 4-aminopyrrolo [2, 1-f] [1, 2, 4] triazine; and 5) reacting the intermediate IV with a bromination reagent to obtain a final product, namely 7-bromopyrrolo [2, 1-f] [1, 2, 4] thiazine-4-amine. The preparation method disclosed by the invention has the advantages of cheap and easily available raw materials, few reaction steps, high yield, mild reaction conditions and capabilityof realizing large-scale production.

The invention relates to the field of emulsion polymerization and discloses a vinyl acetate-acrylate-ethylene multipolymer emulsion and a preparation method thereof. The method comprises the followingsteps: under an emulsion polymerization reaction condition, (1) in the presence of an oxidization-reduction initiating system, carrying out a first polymerization reaction on a part of mixed monomercontaining a vinyl acetate monomer and an acrylate monomer and vinyl monomer, wherein in the oxidization-reduction initiating system, the oxidizing agent is tert-butyl hydroperoxide and the reducing agent is zinc formaldehyde sulfoxylate and / or sodium formaldehyde hyposulfite; and (2) adding the vinyl monomer and residual part of the mixed monomer into the system after the first polymerization reaction for a second polymerization reaction, wherein in the second polymerization reaction, tert-butyl peroxybenzoate is added into the reaction system. The content of acrylics in the copolymer emulsion obtained by the method is obviously higher than those in common modified EVA in the prior art, and the emulsion is good in bonding strength.

The invention discloses a method for preparing (3S)-3-(4-aminophenyl)-piperidyl-1-tert-butyl formate. The method is characterized by comprising the following steps: 1) performing a contact reaction on a 3-(4-aminophenyl)-piperidyl-1-tert-butyl formate racemate and (R)-(-)-binaphthyl-2,2-diyl hydrogen phosphate, cooling, crystallizing, and filtering to obtain a solid compound A; (2) hydrolyzing the solid compound A obtained in the step (1) under an acidic condition, adjusting the pH to be 8 to 10 after the hydrolysis reaction is completed, extracting with ethyl acetate, and concentrating to obtain the (3S)-3-(4-aminophenyl)-piperidyl-1-tert-butyl formate. The method provided by the invention is high in yield and high in product optical purity, and provides a new way for preparing the (3S)-3-(4-aminophenyl)-piperidyl-1-tert-butyl formate.

The invention discloses a thermoplastic acrylic resin coating. Raw materials of the thermoplastic acrylic resin coating comprise, by weight, 100 parts of a thermoplastic acrylic resin, 50-70 parts of xylene, 50-70 parts of n-butanol, 10-15 parts of a coloring pigment, 3-5 parts of a corrosion-resistant pigment, 0.5-1.5 parts of a wetting dispersant and 0.1-0.5 part of a defoaming agent, wherein the thermoplastic acrylic resin comprises, by weight, 100 parts of a mixture obtained by mixing methyl methacrylate and cyclohexyl methacrylate according to a ratio of 1:3, 15-25 parts of methacrylic acid, 25-30 parts of styrene, 25-30 parts of dibenzoyl peroxide, 3-5 parts of dibenzoyl peroxide, azobisisbutyronitrile or tert-butyl peroxybenzoate, 0.5-1.5 parts of triphenylphosphine and 35-50 parts of a mixed solvent obtained by mixing polyvinyl alcohol and water according to a ratio of 1:35-50. The prepared coating can be applied by diluting with an organic solvent, can also be applied by hot melting, and has good adhesive force to surfaces of cement, asphalt and plastics.

The invention provides a preparation method of alkali-soluble solid dispersant resin. The preparation method includes uniformly mixing acrylic acid, styrene, alpha-methyl styrene, maleic anhydride, di-tert-butyl peroxide and / or tert-butyl peroxybenzoate at room temperature to obtain mixture A, adding linear alcohol ethoxylates and solvent diethylene glycol dimethyl ether into a reactor with heating to 140-160 DEG C,adding the mixture A under nitrogen atmosphere, then heating up to 170-185 DEG C for polymerization reaction for 20-60 min, and performing reduced pressure distillation after reaction to obtain the alkali-soluble solid dispersant resin. During mass polymerization of styrene and acrylic acid, the hydrophilic-lipophilic amphiphilic component, namely linear alcohol ethoxylates is added, the terminal hydroxyl group of the linear alcohol ethoxylates reacts with maleic anhydride or acrylic acid in the system to form a hydrophilic-lipophilic side chain, the lipophilic group at the terminal of the side chain changes bonding point distribution of dispersant and pigment, bonding stability of dispersant and pigment is improved beneficially, and dispersing performance on pigment is improved.