47 results about "Trifluoroacetyl chloride" patented technology

The invention relates to an efavirenz intermediate synthesis method, in particular to a synthetic method of 4-chlorine-2-trifluoroacetyl aniline aquo-complex hydrochloride, and belongs to the technical field of medicine intermediate synthesis. The synthesis method comprises the following steps that, at the low temperature, an n-butyllithium solution is added into a 4-chlorine-N-pivalic acyl aniline solution in a dropwise mode, and a 4-chlorine-N-pivalic acyl aniline bi-lithium salt solution is obtained after a reaction is finished; trifluoroacetyl chloride gas is led to the solution at the low temperature to obtain 4-chlorine-2-trifluoroacetyl-N-pivalic acyl aniline; finally, the 4-chlorine-2-trifluoroacetyl-N-pivalic acyl aniline is hydrolyzed on the acidic condition to obtain the product 4-chlorine-2-trifluoroacetyl aniline aquo-complex hydrochloride. According to the method, the n-butyllithium serves as alkali and is basically converted into a lithium chloride solution with the high economic value after being neutralized through hydrochloric acid, recycling is facilitated, and the waste water treatment difficulty can be lowered; the low-price trifluoro-acetylchloride serves as the raw material, and the production cost can be reduced.

2-Trifluoromethyl-5-(1-substituted)alkylpyridines are produced efficiently and in high yield from an alkyl vinyl ether and trifluoroacetyl chloride by cyclization.

The invention relates to a preparation method of compounds, in particular to a method for using trichloroethylene to prepare trifluoro-acetic chloride. The preparation method includes the following steps: (1) 1, 1, 1 three fluorine 2, 2 preparation of dichloroethane: mixed gas is obtained by the trichloroethylene through fluorination and thermal chlorination; the mixed gas enters a reaction tank filled with activated carbon for catalytic chlorination; the reaction temperature is 180-240 DEG C; the speed ratio of controlling chlorine and the mixed gas in a reaction catalysis process is 1:10-80;after reaction, the gas is washed by water alkali and fractionated to obtain products; (2) preparation of the trifluoro-acetic chloride. The preparation method of the method for using the trichloroethylene to prepare the trifluoro-acetic chloride has the advantages of being simple in process, low in cost, high in reaction conversion rate and little in environmental pollution. The method for usingthe trichloroethylene to prepare the trifluoro-acetic chloride requires gas phase space in a reactor and shading components is arranged below a gas-liquid interface. Mercury lamps are completely submerged under the shading components, thereby being capable of effectively preventing TFAC from being radiated and decomposed by the mercury lamps in the gas phase space and avoiding a corrosion problemof decomposition products to a glass reactor and lamp tubes.

The invention relates to a method for continuously synthesizing trifluoroacetyl chloride and sulfuryl fluoride, which comprises the following process: continuously introducing sulfur trioxide and trifluorotrichloroethane (F113a) into a reaction rectifying tower containing a catalyst and a filler thorough the lower part in the tower according to a mol ratio of 1:1, wherein the temperature of the tower is controlled to range between 120 DEG C and 130 DEG C, and the reflux ratio at the top of the tower is 2.5-3; introducing tower bottoms into a sulfuryl chloride separating tower for rectification and separation, wherein the tower temperature is 145-150 DEG C, and the reflux ratio is 0.5-1.0; returning pyrosulfuryl chloride in the separating tower to the middle upper part of the reaction rectifying tower, heating the sulfuryl chloride rectified off from the top of the tower to 150 DEG C, and then introducing the rectified sulfuryl chloride and preheated recycled and newly-added hydrogen fluoride gas into a reactor containing a palladium / charcoal catalyst, wherein the reaction temperature is controlled to range between 150 DEG C and 160 DEG C; separating out unreacted hydrogen fluoride from the reaction product through a cold trap, and returning to the reactor for further use; and then absorbing and separating hydrogen chloride through a falling film, drying, compressing, and condensing to obtain the sulfuryl fluoride. The invention has the advantage of easy acquisition of raw materials, and the sulfuryl chloride byproduct can be directly used for the synthesis of sulfuryl fluoride.

4-Chloro-4-alkoxy-1,1,1-trifluoro-2-butanones, prepared by reacting alkyl vinyl ethers with trifluoroacetyl chloride, are useful for preparing 4-alkoxy-1,1,1-trifluoro-3-buten-2-ones.

The invention discloses a synthesis method of 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-one, which comprises the following steps: adding absolute ethyl alcohol, mercury acetate and n-butyl vinyl ether into a reaction flask which is provided with a fractionating column (connected with a condenser and cooled by an ice salt bath for the flask), heating and refluxing, controlling the temperature of the top of the fractionating column to 36-37 DEG C, evaporating out ethyl vinyl ether, and cooling to obtain the 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-one, namely the 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-one. The preparation method comprises the following steps: mixing ethyl vinyl ether and trifluoroacetic anhydride, adding a deacidification agent, and reacting at 50-110 DEG C for 2-4 hours to obtain the 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-ketone. According to the method, trifluoroacetic anhydride is adopted to replace trifluoroacetyl chloride to serve as a reaction raw material, trifluoroacetic anhydride is easy to prepare and convenient to obtain, and large-batch production of 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-ketone is facilitated.

The invention provides a benzylthio acetamido acetylpyrazine triazole derivative. A target compound (I) is obtained by condensing a sulfydryl acetamido acetic acid derivative and a benzyl chloride derivative, condensing the condensed derivatives and 2-piperazinone, reacting the obtained condensed product and trimethyloxonium tetrafluoroborate so as to obtain a methoxy imide compound, and carryingout cyclization on the methoxy imide compound and hydrazine, trifluoroaceticanhydride, acetic anhydride, propionic anhydride, trifluoroacetyl chloride, acetyl chloride or acrylyl chloride. The preparation method provided by the invention has the advantages of reasonable design, stable process, easily obtained raw materials for production, no use of high pressure hydrogenation and good production feasibility. By using the benzylthio acetamido acetylpyrazine triazole derivative provided by the invention, dipeptidyl peptidase-IV (DPP-4) can be selectively inhibited; an effect of reducing blood sugar is obtained; and the derivative can be applied to the preparation of drugs for reducing the blood sugar and has the following structural formula (I).

The invention discloses a method for synthesizing trifluoroacetyl tripeptide-2. The method first synthesizes NH by Wang Resin 2 ‑Val‑Tyr(tBu)‑Val‑Wang Resin resin peptide, and then the resin peptide and 6‑chlorobenzotriazole‑1,1,3,3‑tetramethyluronium hexafluorophosphate, 1‑hydroxy Synthesis of N-(2,2,2-trifluoroacetyl)-Val-Tyr(tBu)-Val-Wang Resin by reaction of benzotriazole, trifluoroacetic acid and N,N′-diisopropylethylamine, and finally It was cut, purified, and freeze-dried to obtain trifluoroacetyl tripeptide-2. The present invention adopts low-cost, simple and easy-to-obtain trifluoroacetic acid to replace expensive ethyl trifluoroacetate or trifluoroacetyl chloride, and simultaneously adopts the process of first activating trifluoroacetic acid and then neutralizing the acidity, thereby overcoming the effect of trifluoroacetic acid on NH 2 The influence of ‑Val‑Tyr(tBu)‑Val‑Wang Resin resin peptide has the advantages of low cost, high efficiency and simple method, and is an ideal method for the synthesis of trifluoroacetyl tripeptide‑2.

The invention discloses a method for preparing 4-(trifluoromethyl)nicotinic acid, and belongs to the technical field of methods for preparing chemical pharmaceutical intermediates. The method comprises steps of using trifluoroacetyl chloride, vinyl ethyl ether and 3-aminoacrylonitrile as raw materials to prepare the 4-(trifluoromethyl)nicotinic acid through acylation, cyclization and hydrolysis reactions. The method provided by the invention is relatively cheap and easily available in adopted raw material, simple and convenient to operate, easy in separation and purification of products in each step, high in yield, and more suitable for industrial production.

The invention belongs to the field of light-curing bio-based intelligent materials, and in particular relates to a preparation method of visible light-curing self-repairing fluorine-containing polyurethane resin. First use dichloromethane, dual active functional group photoinitiator, weakly basic acid-binding agent and trifluoroacetyl chloride to react in a nitrogen protection device to prepare a fluorine-containing photoinitiator; Dicarboxylation treatment, under the synergistic action of dihydroxy fluorine-containing monomer, fluorine-containing photoinitiator and diisocyanate, finally prepares self-healing fluorine-containing polyurethane resin cured under visible light conditions. The polyurethane resin of the present invention overcomes the shortcomings of traditional light-curing resins such as high brittleness, easy damage, and poor high temperature resistance. It is cured by visible light that is friendly to the human body, and the material has a self-repairing function, which can prolong the service life of the material and enhance weather resistance and high temperature resistance. properties, the source of the monomer is renewable, and the application prospect is good.

The invention discloses a preparation method of ethyl trifluoroacetate, which comprises the following steps: 1) passing sulfur trioxide and trifluorotrichloroethane into an oxygenation reactor twice; 2) trifluoroacetyl chloride and By-products and some raw materials enter the stripping kettle for stripping, condensation and separation; 3) The separated trifluoroacetyl chloride is transported to the hydrolysis absorption system, and part of the raw materials are condensed and refluxed to the oxo reactor; 4) The raw materials after rectification are returned to the oxygen reactor. generation reaction kettle; sulfuryl chloride, pyrothionyl chloride and impurities to be hydrolyzed; 5) obtain crude trifluoroacetic acid, and rectify to obtain trifluoroacetic acid; 6) add trifluoroacetic acid to the esterification kettle; 7) obtain ethyl trifluoroacetic acid finished product . The present invention adds reactants in stages, the reaction conversion rate is higher, and lays a good reaction foundation for subsequent reactions. The reaction conditions are mild, the amount of concentrated sulfuric acid is greatly reduced, and the corrosion to equipment is reduced; adding fibers in frozen brine, Separation of trifluoroacetyl chloride is more efficient.