37 results about "Methyl trifluoromethanesulfonate" patented technology

The invention discloses a method for preparing Lacosamide by a one-pot method. The method comprises the steps: subjecting D-serine and an acetylation reagent to a reaction in a manner of taking dichloromethane as a solvent, and adjusting the pH of a reacted substance to 12-13 by an organic base after the reaction ends; then, controlling the temperature to -5 to 0 DEG C, and adding methyl trifluoromethanesulfonate into the reacted substance for a reaction; and cooling a reacted substance to the temperature of -30 to -25 DEG C, adding a dehydrating agent and benzylamine into the reacted substance for a reaction, carrying out depressurized-concentration drying on material liquid after the reaction ends so as to obtain crude Lacosamide, and then, carrying out recrystallization, thereby obtaining pure Lacosamide. The preparation method is simple and easy in operation, and the prepared Lacosamide has the purity of 99.90% or more and the chiral purity of 99.90%.

The invention discloses a preparation method of a 3-aryl-1-indanone derivate. The structural formula of the 3-aryl-1-indanone derivate is shown in the formula III. The preparation method comprises the following steps that a compound shown in the formula I reacts with a compound shown in the formula II in the presence of methyl trifluoromethanesulfonate, and therefore the 3-aryl-1-indanone derivate shown in the formula III is obtained. The preparation method of the 3-aryl-1-indanone derivate is scientific and reasonable, 3-aryl-1-indanone derivates with various substituent groups can be obtained, the raw materials are easy to obtain, no metal participates in the reaction, reaction atoms are economical, and meanwhile the preparation method has the advantages that operation is simple and convenient, the synthesis productive rate is high, the product is easy to purify, and environmental protection is achieved.

The invention provides a method for preparing methyl hesperidin. The method comprises the following steps: enabling hesperidin as a main raw material to react with trifluoro-methyl methanesulfonate inthe presence of an alkali, performing acidification, filtration and desolvation, further washing with an organic solvent, and filtering, thereby obtaining the methyl hesperidin, wherein the purity ofthe methyl hesperidin is 95% or greater, and the yield of the methyl hesperidin is greater than 90%. The byproduct trifluoro-mesylate is a raw material for synthesizing trifluoromethanesulfonic acid.Compared with the prior art, the method for preparing the methyl hesperidin is safe in reaction process, simple and convenient to operate, efficient and environmental-friendly and applicable to industrial production.

The invention discloses a method for improving thermal stability of liquid fructosaminase. The method comprises the following steps: 1) preparing a tris(hydroxymethyl) aminomethane-hydrochloric acid buffer solution comprising fructosaminase and sodium azide and having a pH value of 7.5-8.5; 2) under a low-temperature stirring condition, adding 1-butyl sulfonate-3-methyl trifluoromethanesulfonate, trehalose and TritonX-100 into the buffering solution prepared in the step (1). With adoption of the method disclosed by the invention, the thermal stability of the fructosaminase is obviously improved, and the fructosaminase can be applied to develop a determination reagent for glycated albumin determined by an FAOD (fructosaminase) clearance method; the method for improving thermal stability of liquid fructosaminase cannot interfere GA content determination by the FAOD clearance method, can obviously improve the thermal stability of the liquid for fructosaminase, enables the liquid fructosaminase to be still enough in activity 12 months after preservation at the temperature of 4 DEG C.

The invention discloses a preparation method of a 5-arylsulfonyl-2-chlorophenol compound, which is prepared from a 2-(5-arylsulfonyl-2-chlorophenoxy) pyridine compound as a raw material by the following steps: A: directly adding the 2-(5-arylsulfonyl-2-chlorophenoxy) pyridine compound, methyl trifluoromethansulfonate and toluene into a reacting device, stirring for reacting for 24 hours at 100 DEG C, and then separating a crude product; and B: adding the crude product obtained in the step A to methanol, adding sodium, refluxing for 15 minutes, and separating to obtain the 5-arylsulfonyl-2-chlorophenol compound. The preparation method is simple and mild in reaction conditions, is finished in one step, and can be well applied to preparation of the 5-arylsulfonyl-2-chlorophenol compound.

Disclosed is a meta-position alkylphenol synthesizing method. The meta-position alkylphenol synthesizing method is obtained through direct reaction of 2-(3-alkyl-phenoxy) pyridine and methyl trifluoromethansulfonate. The method comprises a reaction process of directly adding the 2-(3-alkyl-phenoxy) pyridine, the methyl trifluoromethansulfonate and methylbenzene into a reaction device; in a nitrogen atmosphere, performing stirring at 100 DEG C for reaction for 24 hours, and after the reaction is completed, separating out coarse products; adding the coarse products and sodium into methyl alcohol for refluxing for 15 minutes, and then performing separation to obtain meta-position alkylphenol compounds. The meta-position alkylphenol synthesizing method is reliable in raw material source and simple in reaction and is an economic and efficient meta-position alkylphenol preparing method.

The invention discloses a method for preparing methylmercaptodiafenthiuron. The method comprises the following reaction formula described in the specification, wherein in the formula, a methylation reagent is selected from methyl chloride, methyl bromide, methyl benzenesulfonate, methyl trifluoromethansulfonate, methyl p-toluenesulfonate, dimethyl carbonate, trimethyl phosphate, dimethyl sulfate, diazomethane, methyl trichloroethanimidate, and formaldehyde+formic acid; an alkali is selected from M2CO3, NCO3, MHCO3, MXR1, N(XR1)2, MH, NH2 or NO; M is selected from Li, Na or K; N is selected from Mg or Ca; X is selected from O or S; R1 is selected from H or C1-C6 alkyl. The compound shown in the reaction formula undergoes a reaction with the methylation reagent and the alkali in a proper solvent to prepare the methylmercaptodiafenthiuron. According to the method, the methylation reagent with low price is used, so the product cost is reduced; and the method is mild in reaction condition, simple, convenient and feasible in post-treatment method, economic and effective, and prone to industrialized production.

The invention discloses quick-preparation type plant alkaloid insecticidal powder for peach trees and a preparation method of the quick-preparation type plant alkaloid insecticidal powder. the plant alkaloid insecticidal powder is prepared from the following components in parts by weight: 4.534-8.655 parts of 1,2-dicarboxy-propyl carborane, 3.982-9.376 parts of N-bromosuccinimide, 9.456-14.269 parts of cod-liver oil extracts, 4.257-8.657 parts of methyl methacrylate, 1.354-4.156 parts of biscyclopentadienyl iron, 5.698-7.156 parts of acetic p-toluenesulfonic anhydride, 4.598-7.325 parts of divinyltetramethyldisiloxane, 18.657-20.723 parts of alliin, 10.687-15.893 parts of divinyltetramethyldisiloxane, 12.586-17.951 parts of calla extract liquor, 7.635-12.675 parts of methyl trifluoromethanesulfonate, 1.589-7.896 parts of N, N-dimethylformamide, 10.893-16.753 parts of 2-oxo-1-imidazolidinecarbonyl chloride, 8.394-12.756 parts of 3-acetyl-1-chlorocarbonyl-2-imidazolidone, 14.659-18.546 parts of 3-chlorocarbonyl-1-methanesulfonyl-2-imidazolidinone, 4.893-8.885 parts of 1-(2-hydroxyethyl)-2-imidazolidinone, 6.786-10.563 parts of 1-methylsulphonyl-2-imidazolidone, 15.689-22.486 parts of 1,3-dimethyl-2-imidazolidinone, 17.986-22.258 parts of 1-acetyl-2-imidazolidinone and the like and 5.698-8.467 parts of pistia stratiotes extract liquor.

The invention relates to a preparation method of ortho-alkylphenol. A 2-(2-alkylphenoxy) pyridine derivative is used as a raw material to prepare the ortho-alkylphenol. The reaction process includes:directly adding the 2-(2-alkylphenoxy) pyridine derivative, methyl trifluoromethansulfonate and methylbenzene in a reaction device; reacting for 24 h; separating a coarse product; then adding the coarse product in methanol; adding sodium; refluxing for 15 minutes; and separating to obtain the ortho-alkylphenol. The preparation method is simple in route and easy to implement, and side reactions areless in a preparation process.

The invention discloses a preparation method of a flame-retardant anti-static cable material. According to the process, the steps of high-temperature banburying, magnetic stirring, mold casting, stillstanding cooling, water cooling drawing, solid solution aging and the like are respectively performed on active adhesives (prepared from raw materials of vinyltriethoxysilane, polymethylphenyl silicon oil, sodium pyrosulfite, cyclosiloxane fatty ester, dimethyl phthalate, manganese acetate, sodium chromate, hexamine and the like) and raw materials of polyvinyl chloride, polyethylene wax, polyethylene glycol terephthalate, diethylene glycol dibenzoate, ditexanol, dimethoxymethane, sodium p-tolylsulfinate, tricaprylyl citrate, 1-phenyl-1-cyclopentanecarbonitrile, dipropylene aldehyde pentaerythritol, organic phosphite ester, methyl trifluoromethanesulfonate, diammonium phosphate, ammonium chloride and the like to obtain the flame-retardant anti-static cable material. The prepared flame-retardant anti-static cable material has the advantages of good electric chemical performance, anti-static and flame-retardant performance; various user requirements can be met.

The invention is applicable to the technical field of analytical chemistry, and provides a method for detecting methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate residues. The method comprises the steps of dissolving a sample to be detected with alcohol, and fixing the volume to obtain a sample solution; dissolving methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate reference substances with alcohol, and carrying out volume metering to acquire a plurality of reference substance solutions with concentration gradients; sequentially injecting the reference substance solutions and the sample solution according to chromatographic conditions and mass spectrum conditions for analysis to acquire spectrum data; and drawing a linear correlation working curve according to the spectrum data, and calculating the residues of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate in the sample to be detected. The sample treatment process is simple and convenient, alcohol serves as a solvent and a derivatization reagent, the derivatization reaction is mild, rapid and complete, interference of a complex derivatization reagent on detection is avoided, the detection specificity, precision and accuracy are improved, and the method has an important research value in the aspects of bulk drug quality research, impurity analysis and control research and the like.

The invention discloses a synthetic method of O-glycoside. The technical solution is that alcohol is glycosylated in an anhydrous organic solvent by using a reagent combination of 1,3-dibromo-5,5-dimethylhydantoin (DBDMH) and a catalytic equivalent of 4-iodopyridin-N-methyl trifluoromethanesulfonate (IPTF) as activator and thioglycoside as a glycosyl donor to generate the O-glycoside. The method is simple and reliable, and is suitable for large-scale industrial production.

The invention provides a trimethylsilyl trifluoromethanesulfonate preparation method. A reaction route is shown as CF3SO2X+(CH3)3SiOH->CF3SO2OSI(CH3)3+XH, wherein X=OCH3,OC2H5. The preparation methodincludes the production steps: adding methyl trifluoromethanesulfonate or ethyl trifluoromethanesulfonate in a mole ratio of 1:(1.2-4) into trimethyl silanol, adding a small quantity of a catalyst, performing stirring reaction for 1-10 hours at the reaction temperature ranging from -20 DEG C to 100 DEG C in a dry environment, evaporating out newly generated methanol or ethanol during reaction, rectifying a final product, and collecting a fraction at 135-145 DEG C to obtain a product. By adoption of the method, purity reaches 99.5% or above, the raw material trimethyl silanol can be recycled, the newly generated byproduct methanol or ethanol can be used, and environmental friendliness and suitableness for large-scale production are realized.