191 results about "Benzyl cyanide" patented technology

A method for preparing a loxoprofen intermediate comprises the following steps that 1, on the presence of sodium alkoxide, benzyl cyanide and dimethyl carbonate are subjected to methylation in an organic solvent, and 2-(phenyl cyano) sodium propionate is obtained; 2, 2-(phenyl cyano) sodium propionate and dimethyl sulfate react in an organic solvent to obtain 2-(phenyl cyano) methyl propionate; 4, 2-(phenyl cyano) methyl propionate reacts under the alkaline condition to obtain 2-phenyl propionitrile; 4, 2-phenyl propionitrile is hydrolyzed under the alkaline condition, acid is added for acidizing after the reaction to obtain 2-phenylpropionic acid; 5, 2-phenylpropionic acid, hydrobromic acid and paraformaldehyde are mixed and subjected to a bromine methylation reaction under the acidic condition, and 2-(4-tribromomethyl phenyl) propionic acid is obtained.According to the method, a new synthesis route is designed, product selectivity is good, the purity is high, the conversion rate is high, and few by-products are generated; the raw materials are simple and easy to obtain, the production conditions are mild, the process is simple, production cost is low, and pollution is small.

The invention discloses a 4-aroyl-1,8-naphthalimide compound and a preparation method and use thereof, wherein the 4-aroyl-1,8-naphthalimide compound has a structural formula as shown in the specification, R1 is C1-C10 straight chain or branched chain alkyl; and R2 is phenyl, naphthyl, biphenylyl, substituted phenyl, quinary or senary heteroaryl or benzo quinary or senary heteroaryl. The preparation method is as follows: a 4 bromo-1,8-naphthalimide compound is used as a raw material to react with substituted phenylacetonitrile or aromatic ring acetonitrile in an organic solvent in the presence of an alkali catalyst to obtain a 4-aryl acetonitrile-1,8-naphthalimide compound, and then the 4-aroyl-1,8-naphthalimide compound is obtained in the effects of fluoride ions or cyanide ions. The 4-aryl acetonitrile-1, 8-naphthalimide compound is used as a color or fluorescence sensor for detection of the fluoride ions or cyanide ions, and has high sensitivity and high selectivity during identifying of the cyanide ions in a mixed solvent.

The invention discloses a preparation method of a baloxavir marboxil intermediate. The preparation method is characterized by comprising the following steps: (1) substituting 2-bromomethyl-3,4-difluorophenylacetonitrile through sodium thiophenolate in a solvent A to obtain 3,4-difluoro-2-[(thiophenyl) methyl] benzyl cyanide; (2) reacting the 3,4-difluoro-2-[(thiophenyl) methyl] benzyl cyanide obtained in the step (1) with a cyclizing agent in a solvent B, and carrying out cyclization to obtain 7,8-difluoro dibenzo [b,e] thia heptacyclic-11(6H)-ketone; and (3) reducing the 7,8-difluoro dibenzo[b,e] thia heptacyclic-11(6H)-ketone obtained in the step (2) to obtain 7,8-difluoro dibenzo [b,e] thia heptacyclic-11(6H)-alcohol. The reaction steps in the preparation method are reduced to a six-step reaction from a five-step reaction in the prior art, so that the generation of a side reaction is reduced, and the reaction efficiency is improved. The sodium thiophenolate is used for replacing thiophenol with foul smell and high toxicity, and harm to experimenters during the production is reduced.

The invention discloses a method for separating m-ethyltoluene and p-ethyltoluene by extractive distillation. The extractive distillation solvent adopted by the method is a nitrogenous compound, preferably cyanobenzene or benzyl cyanide, and more preferably benzyl cyanide. The method comprises the following steps: introducing an m-ethyltoluene/p-ethyltoluene mixture from the middle of the extractive distillation tower, and introducing an extractive distillation solvent from the tower top; and after carrying out extractive distillation, discharging the m-ethyltoluene from the top of the extractive distillation tower, discharging the rich solvent containing rich p-ethyltoluene from the tower bottom, sending the rich solvent into a solvent recovery tower, discharging the p-ethyltoluene from the top of the recovery tower, and recycling the extractive distillation solvent discharged from the bottom of the recovery tower. The invention has the advantages of low operation energy consumption and high product purity; and the solvent adopted by the method can obviously improve the relative volatility between m-ethyltoluene and p-ethyltoluene, is easy to recycle, and has high chemical thermal stability.

The present invention discloses a cotesia plutellae kurdjumov attractant and a preparation method thereof, wherein liquid paraffin is adopted as a solvent, and 100 mul/ml benzaldehyde, farnesene, phenylacetonitrile, cis-3-hexenol, trans-2-hexenal, eucalyptol and nonanal are subjected to the same ratio mixing to obtain the attractant. The attractant is specific component screened from plant volatile substances, and has characteristics of high selectivity and strong targeting property. With the attractant, cotesia plutellae kurdjumov early enters a target prevention and control field, enters a search state, and do not flee so as to enhance host search and attack efficiency, increase parasitism rate, and provide important importance for cotesia plutellae kurdjumov pest controlling effect increase, vegetable field pest management improvement and the like.

The invention provides a preparation method for D, L-phenylglycine and an analogue thereof. According to the method, benzaldehyde, an analogue thereof and hydrocyanic acid are adopted as raw materials and subjected to cyanidation reaction, and then 2-hydroxy-benzyl cyanide or 2-hydroxy-benzyl cyanide analogue (cyanohydrin for short) is generated. Cyanohydrin reacts with carbon dioxide and the aqueous solution of ammonia, and then 5-phenyl-hydantoin and an analogue thereof (hydantoin for short) are generated. hydantoin is successively subjected to steam stripping, alkaline hydrolysis, steam stripping, decolorization, neutralization, crystallization, washing, centrifuging, drying and the like to obtain D, L-phenylglycine and the analogue thereof. Compared with the prior art, the preparation method for D, L-phenylglycine and the analogue thereof can significantly and effectively reduce the pollution, and fewer inorganic salt by-products are generated. Meanwhile, the prepared D, L-phenylglycine and the analogue thereof are high in product yield and high in purity. Counted in benzaldehyde and the analogue thereof, the yield of D, L-phenylglycine and the analogue thereof is larger than or equal to 96%, and the product purity is larger than or equal to 99%. Meanwhile, the process flow is simple and feasible, so that the method is worthy of market popularization and application.

The invention relates to a synthesis method for 4-methoxy-2-methyl benzyl cyanide. The synthesis method takes 3, 4-dimethylphenol which is cheap and simple and easy to purchase as the raw material, and comprises six steps: methylation, oxidation, Witting reaction, alkene ether hydrolysis, oximation and dehydration. The synthesis method uses the simple and cheap raw material, is simple to operate, is easy for industrial production, has short production cycle, only needs purification in the last step of the six so as to obtain high-quality 4-methoxy-2-methyl benzyl cyanide, and avoids using extremely toxic substances like NaCN and KCN, thus filling the blank home and abroad.

The present invention discloses the preparation process of 2-fluoro-5-trifluoromethyl benzyl cyanide. The preparation process includes the halogenomethylation of p-fluoro trifluoro toluene to produce 2-fluoro-5-trifluoromethyl benzyl halide, and the nitrilation of 2-fluoro-5-trifluoromethyl benzyl halide to produce 2-fluoro-5-trifluoromethyl benzyl cyanide. The present invention has high yield, low cost and high product purity.

The invention relates to a preparation containing: (i) a composition containing (a) one, two or a plurality of compounds selected from the group consisting of (a1) alcohol monoterpenes of formula (I) in which R1 is H or methyl, R2 is H or C₂-alkenyl, and R3 is a linear or branched, saturated or unsaturated hydrocarbon radical with 4 to 10 carbon atoms, and the enantiomers, diastereomers, racemates, solvates and physiologically compatible salts thereof, and/or (a2) bicyclic epoxy-monoterpenes, (b) at least two lactones of formula (II) in which R4 is H or methyl, R5 is a linear or branched, saturated or unsaturated hydrocarbon radical with 2 to 10 hydrocarbon atoms and n is the number 1 or 2, and the enantiomers, diastereomers and racemates thereof, (c) one, two or a plurality of solvents selected from the group consisting of ethanol, water, dipropylene glycol (DPG), diethyl phtalate (DEP), propylene glycol (PG), isopropyl myristate (IPM), isopropyl palmitate (IPP), triethyl citrate (TEC), triacetin (TRI), 1,2-Propanediol, 1,3-Propanediol, Propanethiol, Pentanediol, Hexanediol, Octanediol, Decanediol (SymClariol®), Dodecanol, 4-hydroxy-acetophenone (SymSave® H), glycerine, butylene glycol, pentylene glycol, hexylene glycol, decylene glycol, propylene carbonate, butylene carbonate, glycerine carbonate, 2-5 benzyl heptanol, lauryl alcohol, trimethyl-hydroxypentyl-isobutyrate, glyceryl-caprylate, ethylhexyl glycerine, benzyl benzoate (BB), and optionally (d) other flavouring agents or aromatic substances selected from the group consisting of 3-phenylbutanal (Trifernal), acetyl methyl carbinol, anethole, anisyl acetate, dihydroeugenol, linalyl formate, 2-methyldecanal, 2-benzyl-2-methylbut-3-ene nitrile (Ci-trowanil® B), 3-hexenyl acetate, styrallyl acetate, belanis, citronellal, cinnamyl acetate, rhubafuran, beta-ions, anther, prenyl acetate, 2-phenyl propanal, 4-(4-hydroxyphenyl)butan-2-one (Frambinon®), ethyl phenoxyacetate, isoralderine, gamma-terpinene, limonene, neocyclocitral, methyl lavender ketone, styrallyl propionate, phenyl ethyl propionate, limonenal, 4-isopentylcyclohexanol (Symrose®), 4-methyl-2-phenyl-3,6-dihydro-2H-pyran/4-methylene-2-phenyl-tetrahydropyrane (Rosyrane super), hydrocitronitril, phenoxanol, isoamyl phenylacetate, damascone, silvial, nectaryl, ambroxide, acetyl pyrazine, trimethyl pyrazine, isoamyl acetate, para-cresyl methyl ether, filbertone, cyclohexyl acetate, heliotropin, acetophenone, anisaldehyde, para-methyl acetophenone, veratraldehyde, methyl anisate and vertoprenal; (ii) aldehydes of formula (III) in which R6 is a saturated or non-saturated, linear hydrocarbon radical; and/or (iii) free fatty acids of formula (IV), in which R7 is a linear or branched, saturated hydrocarbon radical.

The invention discloses a synthesis method for 2-bromine-4-nitryl phenylacetonitrile. The synthesis method uses phenylacetonitrile as a main starting material and comprises the following: 1) a step of nitrifying: stirring the phenylacetonitrile in mixed acid consisting of concentrated sulfuric acid and concentrated nitric acid to react, putting the obtained reaction product in ice water, separating out solid for filtering to obtain precipitate, and then washing the precipitate by water and drying the precipitation in turn to obtain n-nitro-phenylacetonitrile; and 2) a step of bromizing: dissolving the n-nitro-phenylacetonitrile in the concentrated sulfuric acid, adding N-bromosuccinimide to bromize, putting the obtained reaction mixture in the ice water, separating out solid for filtering to obtain precipitate, and then washing the precipitate by water and drying the precipitate in turn to obtain the 2-bromine-4-nitryl phenylacetonitrile. The 2-bromine-4-nitryl phenylacetonitrile synthesized by the method has the characteristics of simple technique, low cost and high yield.

The invention discloses a diazosulfide benzyl cyanide derivative and a preparation method and application thereof. The preparation method for the derivative comprises the following steps that triphenylamine boric acid, diazosulfide and a benzyl cyanide derivative are taken as raw materials and are subjected to Suzuki coupling and Knoevenagel condensation reactions successively to synthesize the target product diazosulfide benzyl cyanide derivative, namely a force-induced fluorescence enhancement material. The color of the material changes under stimulation of lower pressure (the Mpa level), and the material has the advantages that the contrast ratio is high, and fluorescence intensity is improved significantly (the quantum efficiency is improved to 19.3% from 9%), and can be applied to a pressure sensing system.

The present invention discloses a no-catalysis hydrolysis preparation method of benzeneacetic acid with benzyl cyanide in critical water mediator. The method includes the following procedures that: firstly deionized water and benzyl cyanide are added into a high-pressure reactor with the mass ratio of 2:1-8:1, the mixture is agitated openly and the temperature is raised up to boiling point under the normal pressure, then the exhaust valve is kept open for 2-5 minutes; secondly the exhaust valve is kept closed, and the temperature is continuously raised up to 240 DEG C to 310 DEG C for hydrolysis for 1-8 hours; thirdly the hydrolysate is cooled down and crystallized, and crude benzeneacetic acid is obtained; fourthly the crude benzeneacetic acid is decolored with active carbon, secondarily crystallized and dried in vacuum to obtain the product of benzeneacetic acid. The present invention has no need to add any catalyst during the reaction process, thereby solving the puzzle of pollution of catalyzed hydrolyzation of acid and alkali, and having the advantages of simple process, green operation, high purity and high yield.

The invention relates to a fluorescence probe for detecting cyanide ions and a preparation method and application of the fluorescence probe. The fluorescence probe is a cyanide ion fluorescence probetaking boron dipyrromethene (BODIPY) as a fluorescence signal group and taking an activated CH group in a benzyl cyanide group as a recognition site, and the probe is obtained through a nucleophilic substitution reaction of 3,5-dibromo8-phenyl boron fluoride dipyrrole and benzyl cyanide. Through the research of an ultraviolet absorption and a fluorescence emission spectroscopy method, it is foundthat the probe can identify the cyanide ions singly, the lowest detectable limit in a 70% aqueous solution can reach 148 nM, and the recognition process is not disturbed by other anions. Compared withthe prior art, the fluorescence probe has the advantages that the synthesis method is simple, the raw materials are easy to obtain, the cost is lower, the selectivity to the cyanide ions is good, thesensitivity is high, reversibility is provided, the detection can be performed in the aqueous solution, and therefore the fluorescence probe has a good application prospect in the detection of the cyanide ions.

The invention relates to a method for synthesizing a repaglinide key intermediate, namely 4-ethoxycarbonyl-3-ethyoxy phenylacetic acid. The method comprises the following steps: by taking 3-ethyoxy-4-ethoxycarbonyl-benzyl cyanide as an initial raw material, performing hydrolysis, esterification, selective hydrolysis and the like, thereby obtaining the important intermediate 4-ethoxycarbonyl-3-ethyoxy phenylacetic acid of repaglinide. According to the key intermediate, the impurities of the product is less, the purity of the product is high and can reach over 99.7%, so that the quality of the subsequently synthesized repaglinide product is improved, the 100 percent first-pass yield of the subsequently synthesized repaglinide product can be basically reached, a refining step is avoided, and the synthetic yield is effectively improved. The process is easy and convenient to operate, the yield is high, the molar yield is 69.1 percent, the production cost is low, and the method is suitable for industrial production.

The invention discloses a method for synchronizing m-benzenyl trifluoride di-cyan acetonephenone which is an important intermediate for metaflumizone, a kind of efficient insecticide. The method includes utilizing 4-cyanobenzylchloride as raw materials to generate 4-cyano phenylacetonitrile to be reacted with methyl 3-benzoate in organic solvent for 5-8 hours. The yield of the intermediate of the metaflumizone produced by the method is higher than 90%, and content is higher than 89%. The method for synchronizing m-benzenyl trifluoride di-cyan acetonphenone is high in yield, low in cost and can be used for industrial production.

The invention provides a preparation method for a fosamprenir intermediate. The preparation method comprises the following steps: taking benzyl cyanide as a raw material, and performing steps of nitrile hydrolysis, acylation, reaction with a Grignard reagent, ammonization, cyclizing and the like for synthesizing (2R,3S)-1,2-epoxy-3-t-butyloxycarborylamino-4-phenyl butane. The method is reasonable in process, simple to operate, low in cost and high in yield; with the method, industrialization can be well realized and the production efficiency is improved.

The invention relates to a process for preparing 3-amino phenylacetic acid with p-nitro benzyl cyanide as raw materials, by reduction, acetylation, nitrification, hydrolysis, esterification, deamination, reduction and hydrolysis. The invention has high selectivity and the raw materials are cheap and easily available.

The invention discloses a preparation method of phenylacetic acid, which comprises the following steps of: 1) heating benzyl cyanide to 50-100 DEG C, dropwise adding hydrochloric acid to the benzyl cyanide or dropwise adding the molten benzyl cyanide to hydrochloric acid, wherein the molar ratio of the hydrochloric acid to the benzyl cyanide is (1.2-5):1; after dropwise adding, performing a heat preservation reaction for 1-5 hours; and ending the reaction when the mass content of the benzyl cyanide in the reaction system is less than 5%; and 2) performing reduced-pressure distillation for recovering the unreacted benzyl cyanide in the reaction system of the step 1) until the mass content of the benzyl cyanide in the reaction system is less than 0.2%; adding water to the reaction system, and stirring and mixing; cooling for crystallization and performing suction filtration; and washing the obtained crystal with water, and drying to obtain a phenylacetic acid product. According to the preparation method disclosed by the invention, a technology of directly hydrolyzing benzyl cyanide with hydrochloric acid to prepare phenylacetic acid is adopted, few kinds of reactants are used, other organic matters except the raw material benzyl cyanide are not required, the consumption is low, the after-treatment is simple, and both the appearance and quality of the product meet requirements.

The invention belongs to the field of medical chemistry, and in particular relates to a synthesis method of pheniramine maleate. The method includes the following steps: (1) reacting benzyl cyanide with acetylene gas in the presence of a cobaltocene catalyst to generate benzyl pyridine; (2) reacting benzyl pyridine with N,N-dimethyl chloroethane under the catalysis of sodium amide to generate pheniramine, and conducting neutralization reaction on pheniramine with maleate to generate pheniramine maleate.

The invention discloses a method for hydrolyzing phenylacetonitrile in an ammonia-containing high-temperature liquid water medium and preparing phenyl acetamide and phenylacetic acid simultaneously. The method comprises the following steps: 1) deionized water and the phenylacetonitrile with the mass ratio of between 2 to 1 and 8 to 1 are added into a high-pressure reaction kettle, are stirred, and are heated to boil, and an exhaust valve is opened for 2 to 5 minutes; 2) 25 percent ammonia water is pumped through a metering pump to ensure that the ammonia concentration in reactants in the kettle is between 0.05 and 4g/L, and the temperature is increased to be between 180 and 250 DEG C to hydrolyze for 5 to 120 minutes; 3) the temperature is reduced to recover ammonia gas in the kettle; 4) a hydrolysate is cooled, the pH value of the hydrolysate is adjusted to between 8 and 9 , and the hydrolysate is crystallized, and filtered to obtain crude phenyl acetamide; 5) the crude phenyl acetamide is subjected to decolorization by activated carbon, secondary crystallization and vacuum drying to obtain a phenyl acetamide product; and 6) the pH value of filtrate in step 4) is adjusted to between 3 and 4, and the filtrate is crystallized to obtain crude phenylacetic acid, and then the crude phenylacetic acid is subjected to decolorization by the activated carbon, secondary crystallization and vacuum drying to obtain a phenylacetic acid product. The method has a simple and environment-friendly technical process.

The invention discloses an air catalytic oxidation treatment benzyl cyanide waste water method. Active carbon serves as promoter and copper sulfate solution serves as a main catalytic agent to soak the active carbon to prepare composite catalyst which is filled in an air oxidation tower. Benzyl cyanide waste water after pretreatment enters the tower from the upper portion of the tower, air is led in from the lower portion of the tower, the waste water and the air are in countercurrent contact, and water after treatment flows out form the lower portion of the tower. Copper sulfate solution with mass fraction of 15% is prepared, the copper sulfate is infiltrated in the air oxidation tower to spray and soak the activated carbon, and moisture is dried for reserve through lead-in air. The benzyl cyanide waste water after pretreatment is infiltrated in a head tank, oil water is separated again at normal temperature after settling separation, the air is led in, and airflow is kept to be stable for 10min. The benzyl cyanide waste water after pretreatment is added in an air oxidation tower, water after pretreatment is observed, the water is colorless and transparent, cyanide ion content in the water after treatment is detected, when the cyanide ion content is smaller than 0.5mg/L, the waste water is qualified, on the contrary, the waste water is disqualified. The qualified water is discharged or enters a next working procedure for comprehensive utilization.