90 results about "O-nitrobenzaldehyde" patented technology

The present invention is preparation process of nifedipine and relates to the field of organic chemical technology. Under the action of pyridine carboxylate in the catalytic amount, o-nitrobenzaldehyde and methyl acetoacetate are made to react to produce intermediate benzylidene compound, which is reacted with methyl acetoacetate and ammonia directly to produce nifedipine. In o-nitrobenzaldehyde,the total yield of re-crystallized nifedipine may reach 70%.

The invention provides a preparation method for an o-nitrobenzaldehyde compound. The method directly taking benzaldehyde compounds as starting raw materials comprises the following steps: firstly, converting a formyl group into an O-methyl oximido; secondly, taking divalent palladium salt as a catalyst, and realizing the carbon-hydrogen bond activation single nitration reaction on an o-position of an oximido under the condition that both an oxidant and a nitration agent exist; finally, removing the O-methyl oximido by using strong organic acid to obtain the o-nitrobenzaldehyde compound. The nitration method provided by the invention has the advantage of specificity in the o-position of a nitration position, the reaction process is safe and environment-friendly, the substrate is excellent in adaptability, and various substituents can realize o-position nitration; various benzaldehyde is directly taken as raw materials, so that the reaction steps are simple, and the synthesizing method is a novel route for synthesizing various o-nitrobenzaldehyde compounds containing substituents.

The present invention is preparation process of nifedipine and relates to the field of organic chemical technology. Under the action of pyridine carboxylate in the catalytic amount, o-nitrobenzaldehyde and methyl acetoacetate are made to react to produce intermediate benzylidene compound, which is reacted with methyl acetoacetate and ammonia directly to produce nifedipine. In o-nitrobenzaldehyde, the total yield of re-crystallized nifedipine may reach 70%.

The invention discloses a method for synthesizing o-aminobenzaldehyde. The method comprises the following steps: adding a Pd / C or Ni / C catalyst into a mixed solvent containing o-nitrobenzaldehyde; replacing air in a high-pressure reaction kettle with N2, and introducing H2 to react at 50-120 DEG C for 5-10 hours; filtering reaction liquid, and analyzing filtrate by virtue of a high performance liquid chromatography, wherein the conversion rate and the selectivity can reach 90% or more. According to the method, the catalyst can be recycled after the reaction; no waste liquid and waste residue is emitted in the reaction process; aldehyde is not reduced when nitryl is reduced.

The invention relates to a process for preparing aromatic aldehydes, in particular a process for preparing o-nitrobenzaldehyde through bionic catalytic oxidation of ortho-methylnitro benzene, wherein metallic phthalocyanine, single nuclear metalloporphyrin or mu-oxy-double nuclear metalloporphyrin having the similar structure as the biological enzymes are selected as the catalyst for the disclosed process, whose dose is 0.2-1.0% weight of ortho-methylnitro benzene, and methyl alcohol is used as solvent, 0.8-3.0 MPa oxygen is let into 3.0-6.0 mol / L strong alkaline methyl alcohol solution, the reaction temperature is controlled between 25 deg. C to 60 deg. C, the reaction time being 6-48 hrs.

The invention relates to a process for preparing aromatic aldehydes, in particular a process for preparing p-nitrobenzaldehyde through bionic catalytic oxidation of p-nitrotoluene, wherein metallic phthalocyanine, single nuclear metalloporphyrin or mu-oxy-double nuclear metalloporphyrin having the similar structure as the biological enzymes are selected as the catalyst for the disclosed process, whose dose is 0.1-1.0% weight of p-nitrotoluene, and methyl alcohol is used as solvent, 0.5-3.0 MPa oxygen is let into 0.7-2.8 mol / L strong alkaline methyl alcohol solution, controlling the reaction temperature to be 20-65 deg. C, the reaction time being 6-48 hrs.

The invention belongs to the technical field of organic chemistry, and particularly relates to a method for efficiently synthetizing pyrazol[1,5-c]-quinazoline skeleton compounds under no catalytic condition. The structure of the compounds is represented and confirmed with 1H NMR, 13 C NMR, MS and other methods. The method disclosed by the invention comprises the following steps: reacting 1,3-dipolar quinazoline dipoles obtained from o-nitrobenzaldehyde and a series of compounds of triethyl orthoformate with beta-nitrostyrolene under the condition of no any catalysts based on DMSO as a solvent at the temperature of 110 DEG C to generate a series of pyrazol[1,5-c]-quinazoline derivatives. By adopting the method, the pyrazol[1,5-c]-quinazoline compounds can be efficiently prepared. The method disclosed by the invention is mild in reaction conditions and simple to oeprate, the cost is greatly lowered with comparison to the cost of previous reaction between the 1,3-dipolar quinazoline dipoles and terminal alkyne, the reaction conditions are environmentally friendly, the production purity is high, separation and purification are convenient, the method is suitable for large-scale preparation, and the pyrazol[1,5-c]-quinazoline skeleton compounds have excellent application prospect in new drug research and development since the structure of quinazoline compounds has broad-spectrum biological activity.

The invention discloses a preparation method of a 3-alkenyl quinoline-2 (1H) ketone derivative, which comprises the following steps: carrying out reaction on palladium acetate, tris (3-methoxyphenyl) phosphine, carbonyl molybdenum, cesium carbonate, tetrabutylammonium iodide, o-nitrobenzaldehyde and allyl aryl ether at 100 DEG C for 30 hours, and after the reaction is completed, carrying out post-treatment to obtain the 3-alkenyl quinoline-2 (1H) ketone derivative. According to the preparation method, o-nitrobenzaldehyde is used as a nitrogen source and a formyl source, the operation is simple, the reaction initial raw materials are cheap and easy to obtain, the tolerance range of substrate functional groups is wide, and the reaction efficiency is high. Various 3-alkenyl quinoline-2 (1H) ketone derivatives can be synthesized according to actual needs, and the practicability of the method is widened while the operation is convenient.

A computer keyboard disinfection cleaning solution comprises, by weight, 6-10 parts of lemon extracting solution, 3-8 parts of anion surface active agent, 3-6 parts of polytetrahydrofuran ether, 1-4 parts of glutaraldehyde, 0.5-2 parts of essence, 4-6 parts of sodium tripolyphosphate, 1-5 parts of sodium gluconate, 2-4 parts of citric acid, 3-5 parts of ethanediol, 0.6-2.2 parts of emulgator, 2.5-7 parts of o-nitrobenzaldehyde and 25 parts of water. The computer keyboard disinfection cleaning solution has the advantages that equipment can be well sterilized and disinfected through the disinfection cleaning solution, normal usage of the electronic device cannot be corroded or affected, and the disinfection cleaning solution is natural and friendly to the environment.

The invention discloses a synthesis method for an o-Nitrobenzaldehyde compound which is showed in formula I. The method has the following steps: leading a halogenated 2-nitrobenzenemethanol showed in formula II to carry out oxidation reaction with a mixed oxidant of a 2, 2, 6, 6-tetramethylpiperidinooxy and an iodosobenzen ediacetate. The method of the invention is simple in operation, and the reaction condition is gentle, which is not only suitable for small-scale production in laboratory, but also suitable for large-scale industry production, wherein, X relates to Cl, Br, I or F, which is in a third, fourth, fifth or sixth place.

The invention discloses a preparation method of o-nitrobenzaldehyde, wherein the preparation method comprises the following steps: (1) adding o-nitrobenzyl alcohol, a catalyst, a bromide salt and a solvent into a reaction kettle, and uniformly stirring at room temperature; (2) controlling the reaction temperature, slowly dropwise adding a sodium hypochlorite solution into the reaction kettle, and simultaneously adding a weakly alkaline substance or an acidic substance to control the pH value of the reaction; (3) standing for layering, adding an organic solvent to extract a product, and concentrating to obtain a crude product; and (4) crystallizing by using an organic solvent, centrifuging, and drying in vacuum to obtain o-nitrobenzaldehyde. According to the method, 2-(2,2,6,6-tetramethylpiperidine nitroxide radical-4-subunit) acetic acid which is low in price and easy to obtain is used as a catalyst, the sodium hypochlorite solution is used as an oxidizing agent, a mixed solvent of water and chlorinated hydrocarbon is used as a reaction solvent, the o-nitrobenzaldehyde is prepared through oxidation under the mild temperature condition, the raw materials are low in price and easy to obtain, the reaction time is short, the reaction selectivity is high, and the yield is high.

The invention provides a preparation method of methyl 2-nitrobenzal acetoacetate, which comprises the following steps: (1) reacting initial raw materials o-nitrobenzaldehyde and methyl acetoacetate with methanol under the action of a catalyst to generate a compound methyl 2-nitrobenzal acetoacetate; (2) after carrying out vacuum concentration to remove the back, adding a crystallizing solvent, and stirring at low temperature to generate the methyl 2-nitrobenzal acetoacetate solid crude product; and (3) recrystallizing the solid crude product to obtain the methyl 2-nitrobenzal acetoacetate pure product of which the purity is higher than 99.5%. The preparation method provided by the invention has the advantages of mild reaction conditions, short reaction time, high yield and environmental protection; the obtained nifedipine has high purity of the impurity methyl 2-nitrobenzal acetoacetate; and the impurity can be accurately positioned by comparison in the nifedipine related substance inspection, thereby having important instruction meanings for researching nifedipine.