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40results about How to "Easy and green post-processing" patented technology

Polysubstituted pyridine derivative and preparation method thereof

The invention discloses a polysubstituted pyridine derivative and a preparation method thereof. The derivative has a structure as shown in specification, wherein R1, R2, R3, R4 and R5 all are any one selected from hydrogen atom, halogen atom, alkyl, aryl, substituted aryl, acyl, amino, nitryl and alkoxy; the invention also discloses a preparation method of the polysubstituted pyridine derivative; the preparation method comprises the following steps: by taking acetyenic ketone and 1-arylethylamine as raw materials, and under the action of appropriate alkali, heating to have a reaction in the solvent to obtain the polysubstituted pyridine derivative as shown in the formula at high yield. The preparation method is mild in reaction condition, short in reaction time, wide in substrate range, high in reaction specifity, high in yield and simple in after-treatment.
Owner:HUAQIAO UNIVERSITY

Preparation method of N-(2-pyridyl/pyrimidyl)indole derivative

The invention discloses a preparation method of an N-(2-pyridyl / pyrimidyl)indole derivative. The preparation method of the N-(2-pyridyl / pyrimidyl)indole derivative comprises the following steps: mixing a 2-substituted phenylaminopyridine / pyrimidine derivative, an alkenyl azide compound, a catalyst, an oxidizing agent, alkali and an organic solvent uniformly, heating to 60 to 80 DEG C under nitrogen or air, performing a cyclization reaction for 18 to 24 hours, cooling to room temperature after the reaction, and performing concentration and column chromatographic purification to obtain the N-(2-pyridyl / pyrimidyl)indole derivative. By the preparation method, the N-(2-pyridyl / pyrimidyl)indole derivative with various substituent groups which cannot be synthesized according to other methods canbe synthesized; furthermore, the used raw materials are easily available, the yield is high, the reaction condition is mild, the reaction time is short, the substrate range is wide, the reaction specificity is high and aftertreatment is simple, convenient and green.
Owner:HUAQIAO UNIVERSITY

Preparation method of trans-trisubstituted alkene derivative

The invention discloses a preparation method of a trans-trisubstituted alkene derivative. The preparation method comprises following steps: 1, an alkali, an alkyne, a palladium catalyst, a ligand, a halogenated aromatic hydrocarbon, a precursor compound, and an organic solvent are introduced into a reaction container, nitrogen gas is adopted for repeat filling, and reaction is carried out for 12 to 36h at 60 to 140 DEG C; 2, a product obtained in step 1 is diluted with Ethyl Acetate, is washed with water, and is separated so as to obtain an organic phase; and 3, the organic phase obtained in step 2 is subjected to drying, filtering, concentrating, and column chromatography or thin-layer chromatography processing so as to obtain the trans-trisubstituted alkene derivative. According to the preparation method, construction of one carbon boron bond is realized in construction of the trans-tri aromatic hydrocarbon-substituted alkenes, excellent zone selectivity is achieved, and the trans-trisubstituted alkene derivative which is not easily synthesized using other methods is synthesized.
Owner:HUAQIAO UNIVERSITY

Preparation method for substituted isocoumarin derivatives

The invention discloses a preparation method for substituted isocoumarin derivatives. The method comprises the following steps: a novel carbon-carbon bond and a carbon-oxygen bond are constructed while a carbon-carbon bond and a carbon-hydrogen bond are cut, a base, dichloro(p-cymene)ruthenium(II) dimer, 2,4,6-trimethylbenzoic acid and sulfur ylide are reacted in an organic solvent, and thereforethe substituted isocoumarin derivatives are prepared. According to the method provided by the invention, the raw materials used in the method are easy to obtain, the yield is high, the reaction conditions are mild, the reaction time is short, the substrate range is wide, the reaction specificity is strong, and the post-treatment is simple and green.
Owner:HUAQIAO UNIVERSITY

Preparation method of 2-amino cinnamyl alcohol ester derivative

The invention discloses a preparation method of a 2-amino cinnamyl alcohol ester derivative. The method comprises the following steps: (1) sequentially adding a palladium catalyst, a ligand, a cocatalyst, an alkali, an amination reagent, halogenated aromatic hydrocarbon, a termination reagent and an organic solvent into a reaction vessel purged by nitrogen, and reacting at 80 DEG C for 24 hours; and (2) cooling the material obtained in the step (1), and sequentially filtering, concentrating and performing thin-layer chromatography or column chromatography to obtain the product. According to the invention, different aryl-substituted 2-amino cinnamyl alcohol ester derivatives can be obtained at the same time, and a specific E-configuration 2-amino cinnamyl alcohol ester product with good stereoselectivity, which is not easy to obtain by other methods, can be synthesized without additionally adding silver salt; and the method has the advantages of high yield, mild reaction conditions, simple operation steps, wide substrate range, and simple and green post-treatment.
Owner:HUAQIAO UNIVERSITY

3-hydroxy isoindole-1-ketone derivative and preparation method thereof

The invention discloses a preparation method of a 3-hydroxy isoindole-1-ketone derivative (formula 2). A compound as shown by formula (1) is used for carrying out substitution reaction in a solvent in the presence of alkali and air to obtain the 3-hydroxy isoindole-1-ketone derivative. According to the method disclosed by the invention, the oxygen in the air is taken as an oxygen source, the used raw materials are easy to obtain, the yield is high, the reaction condition is mild, the substrate range is wide, the reaction specificity is strong, and the post-processing is simple, convenient and green.
Owner:XIAMEN HUAXIA UNIV

Preparation method of C-aryl glucoside compound

The invention discloses a C-aryl glucoside compound preparation method, which comprises: (1) sequentially adding an alkali, a co-catalyst, a palladium catalyst, a ligand, aryl halide, glycosyl chloride, a termination reagent and an organic solvent to a reaction container subjected to nitrogen purging, and carrying out a reaction for 15-30 h at a temperature of 80-120 DEG C to obtain a mixed material; (2) diluting the mixed material obtained in the step (1) with ethyl acetate, washing with water, and separating to obtain an organic phase; and (3) drying the organic phase obtained in the step (2), filtering and concentrating the organic phase, and carrying out thin-layer chromatography or column chromatography to obtain the C-aryl glycoside compound. According to the method, different aryl-substituted C-aryl glucoside compounds can be obtained, the steps are simple, the operation is safe, the stereoselectivity is good, and the C-aryl glucoside compounds which are difficult to obtain by other methods can be synthesized.
Owner:HUAQIAO UNIVERSITY

Preparation method of polysubstituted azatricycloazine derivative

The invention discloses a preparation method of a polysubstituted azatricycloazine derivative. The preparation method comprises the following steps: after uniformly mixing substituted aminopyridine, acetylene dicarboxylate, a catalyst, a ligand, an oxidant and an organic solvent, heating under an air atmosphere and carrying out cyclization reaction; after the reaction is finished, cooling to roomtemprature to obtain the polysubstituted azatricycloazine derivative. According to the preparation method, the azatricycloazine derivative with various substituent groups, which cannot be synthesizedby other methods, can be synthesized. The cheap metal catalyst is adopted; the preparation method has the advantages of easiness for obtaining the raw materials, high yield, moderate reaction conditions, short reaction time, wide substrate range, strong reaction specificity, simplicity and convenience for post-treatment and greenness.
Owner:HUAQIAO UNIVERSITY

Preparation method of 2,5-disubstituted furan derivatives

The invention discloses a preparation method of 2,5-disubstituted furan derivatives. One carbon-carbon bond is cut off, at the same time, a novel carbon-carbon bond is established, cyclization reactions are carried out to obtain the 2,5-disubstituted furan derivatives, which have good regioselectivity. The method has the advantages of easily available raw materials, high yield, mild reaction conditions, short reaction time, wide substrate range, strong reaction specificity, and convenient and green post-treatment.
Owner:HUAQIAO UNIVERSITY

Polysubstituted 2-hydroxy-1,4-benzoxazine derivative

The invention discloses a polysubstituted 2-hydroxy-1,4-benzoxazine derivative, which has a structural formula shown as in the description. The polysubstituted 2-hydroxy-1,4-benzoxazine derivative which cannot be synthesized by other methods is synthesized; the profound significance is realized in the aspects of organic synthesis and medicinal chemistry; the raw materials used by the method are easily obtained; the yield is high; the reaction conditions are mild; the reaction time is short; the substrate range is wide; the reaction specificity is high; the post treatment is simple and convenient and achieves an environment-friendly effect.
Owner:HUAQIAO UNIVERSITY

A kind of preparation method of 1,2-substituted benzimidazole derivatives

The invention discloses a preparation method of a 1,2-substituted benzimidazole derivative. The preparation method comprises the following steps: uniformly mixing an N-phenyl amidine derivative, a nitrine derivative, an acid compound, a catalyst, a metal salt and an organic solvent; and performing a reaction for 10-13h at 78-82 DEG C in an air atmosphere to obtain the 1,2-substituted benzimidazole derivative. The method disclosed by the invention can be used for synthesizing a compound with a benzimidazole derivative framework, which cannot be synthesized by other methods. The used raw materials are easily available, and the preparation method is high in yield, mild in reaction condition, wide in primer range, small in catalyst dosage, strong in reaction specificity and simple and green in post-treatment, and the utilization ratio of atoms reaches up to 90% and above.
Owner:HUAQIAO UNIVERSITY

A kind of preparation method of 2,4-disubstituted pyrrole derivatives

The invention discloses a preparation method of a 2,4-di-substituted pyrrole derivative. The reaction equation is shown in the description. By adopting the method, a pyrrole derivative with a plurality of substituents which is difficult to obtain with other methods can be synthesized.
Owner:HUAQIAO UNIVERSITY

A kind of synthetic method of quinazolinone aromatic compound

The invention discloses a synthetic method of a quinazolinone aromatic compound. The synthetic method comprises the following steps: dissolving 2-aryl indole, organic amine / inorganic amine and cuprous bromide in an organic solvent; carrying out reaction for 20-30 hours at 60-120 DEG C in the presence of oxygen; and separating and purifying to obtain the quinazolinone aromatic compound. According to the synthetic method, the raw materials are easily available and the yield is high (99%); the synthetic method is mild in reaction condition, short in reaction time, wide in primer range, strong in reaction specificity and simple and green in post-treatment.
Owner:HUAQIAO UNIVERSITY

Preparation method of cis-N-styryl amide derivative

The invention discloses a preparation method of a cis-N-styryl amide derivative, which comprises the following steps of: (1) mixing an N-phenylethynyl amide derivative, p-methylbenzenesulfonyl hydrazide, alkali and an organic solvent, and reacting at 80-90 DEG C for 12-24 hours; (2) diluting the material obtained in the step (1) with ethyl acetate, washing with water, and separating to obtain an organic phase; and (3) carrying out drying, filtering, concentration and column chromatography or thin-layer chromatography on the organic phase obtained in the step (2) to obtain the cis-N-styryl amide derivative. The prepared cis-N-styryl amide derivative has good chemical selectivity, and when a carbon-carbon triple bond participates in the reaction, a cis-configuration product is preferentially generated in the reduction process.
Owner:HUAQIAO UNIVERSITY

A kind of synthetic method of quinoxaline-2(1h)-ketone C-3 phosphonic acid compound

The invention discloses a synthetic method for a 2(1H)-quinoxalinone C-3 site phosphate compound. The synthetic method includes the following steps: (1) dissolving 2(1H)-quinoxalinone derivatives, a phosphatized reagent and potassium persulfate in an organic solvent, and reacting for 7.7-8.3 h at the temperature of 99-102 DEG C in the air conditions; (2) cooling the reaction product obtained in the step (1) to room temperature, and performing separation and purification, so as to obtain the 2(1H)-quinoxalinone C-3 site phosphate compound. According to the synthetic method, raw materials are easy to obtain, the reaction condition is gentle, the addition of an additive, namely a metal catalyst is not needed, and the yield is high (up to 92%); besides, the range of substrates is wide, the reaction specificity is high, and aftertreatment is simple, convenient and green.
Owner:HUAQIAO UNIVERSITY

Multi-substituted pyridine derivatives and preparation method thereof

The invention discloses a polysubstituted pyridine derivative and a preparation method thereof. The derivative has a structure as shown in specification, wherein R1, R2, R3, R4 and R5 all are any one selected from hydrogen atom, halogen atom, alkyl, aryl, substituted aryl, acyl, amino, nitryl and alkoxy; the invention also discloses a preparation method of the polysubstituted pyridine derivative; the preparation method comprises the following steps: by taking acetyenic ketone and 1-arylethylamine as raw materials, and under the action of appropriate alkali, heating to have a reaction in the solvent to obtain the polysubstituted pyridine derivative as shown in the formula at high yield. The preparation method is mild in reaction condition, short in reaction time, wide in substrate range, high in reaction specifity, high in yield and simple in after-treatment.
Owner:HUAQIAO UNIVERSITY

A kind of multi-substituted 2-hydroxyl-1,4-benzoxazine derivative

The invention discloses a multi-substituted 2-hydroxyl-1,4-benzoxazine derivative, the structural formula of which is as follows: the present invention synthesizes a multi-substituted 2-hydroxyl-1,4-benzoxazine derivative which cannot be synthesized by other methods. Oxazine derivatives have far-reaching significance from the perspectives of organic synthesis and medicinal chemistry, and the raw materials used in the method of the present invention are easy to get, the yield is high, the reaction conditions are mild, the reaction time is short, the substrate range is wide, and the reaction is specific. Strong, easy to post-treatment and green.
Owner:HUAQIAO UNIVERSITY

A kind of preparation method of 1-aminoindole derivative

The invention discloses a preparation method of a 1-amino indole derivative. The method comprises the steps of mixing a phenylhydrazine hydrochloride derivative, a diazo compound, an aldehyde or ketone compound, a catalyst, alkali and an organic solvent evenly; and carrying out condensation reaction in air or nitrogen at 80-100 DEG C for 2-12h to obtain the 1-amino indole derivative. The 1-amino indole derivative which cannot be synthesized by other others can be synthesized, and the used raw materials are available, high in yield, mild in reaction condition, wide in substrate range, high in reaction specificity, and simple and green in aftertreatment.
Owner:HUAQIAO UNIVERSITY

A kind of preparation method of indolo[2,1-a]phthalazine derivative

The invention discloses a preparation method of an indole[2,1-a]phthalazine derivative. According to the preparation method of the indole[2,1-a]phthalazine derivative, the indole[2,1-a]phthalazine derivative which cannot be synthesized by other methods is firstly and directly synthesized by a cascade reaction through relatively simple raw materials without the need to use a precious metal catalystand add an oxidizing agent, the reaction raw materials are easy to obtain, the yield is high, the reaction condition is mild, the reaction time is short, the substrate range is wide, and the post-treatment is simple and green.
Owner:HUAQIAO UNIVERSITY

A kind of preparation method of 1,2,3-trisubstituted-5-trifluoromethylpyrrole derivative

The invention discloses a preparation method of 1,2,3-trisubstituted-5-trifluoromethylpyrrole derivatives, comprising the following steps: (1) combining 1,3-diketone derivatives, sulfur ylides, additives and After mixing the organic solvents, react at 60-100°C for 12-24h; (2) Dilute the material obtained in step (1) with ethyl acetate, and then wash with water to separate the organic phase; (3) Dilute the material obtained in step (2) The obtained organic phase is dried, filtered, concentrated and subjected to column chromatography or thin layer chromatography to obtain the 1,2,3-trisubstituted-5-trifluoromethylpyrrole derivative. The present invention has good regioselectivity in the construction of 1,2,3-trisubstituted-5-trifluoromethylpyrrole derivatives; the raw materials used in the present invention are easy to obtain, the yield is high, the reaction conditions are mild, the reaction time is short, and the substrate Wide range, strong reaction specificity, easy post-processing and green.
Owner:HUAQIAO UNIVERSITY

Polysubstituted isocoumarin derivatives and preparation method thereof

The invention discloses a multi-substituent isocoumarin derivative and a preparation method thereof. According to the preparation method, substituted tert-butyl peroxybenzoate represented by a formula II, 1,2-disubstituted acetylene represented by a formula III, a catalyst, alkali, acid and a solvent are uniformly mixed and are heated under the protection of nitrogen for a cyclization reaction, and a compound represented by a general structure formula I is obtained after the reaction. According to the method, the reaction conditions are mild, the reaction time is short, the substrate range is wide, the reaction specificity is high, the yield is high, the post-processing is simple and convenient, and the multi-substituent isocoumarin derivative which cannot be synthesized with other methods can be synthesized and has a wide application.
Owner:HUAQIAO UNIVERSITY

A kind of synthetic method of quinoxalinone compound

The present invention is to dissolve the chloroimine substrate in the addition of Na 2 CO 3 In the dichloroethane solution, under the catalysis of palladium trifluoroacetate, the reaction is carried out in an oil bath for 6-20 h. According to the different functional groups carried by the chloroimine substrate, the reaction atmosphere under the oil bath reaction conditions is different: Imine substrate with CO attached 2 When the Et group is used, the reaction atmosphere is argon, and when the chloroimine substrate is attached to an aryl group, the reaction atmosphere is air. After the completion of the reaction, through thin layer chromatography (TLC) detection, the reaction solution was saturated NH 4 Quenched with aqueous Cl solution, extracted with ethyl acetate, anhydrous Na 2 SO 4 After drying, the solvent was removed, and the quinoxalinone compounds were obtained by column chromatography.
Owner:NINGXIA UNIVERSITY

Multi-substituted 2-pyrrole pyridine derivatives and preparation method thereof

The invention discloses a polysubstituted 2-pyrrolopyridine derivative. The derivative has a structure shown in a formula in the specification, wherein in the formula, R1, R2, R3, R4, R5, R6, R7 and R8 are selected from any one of hydrogen atoms, halogen atoms, alkyl, aryl, substituted aryl, acyl, amino, nitro and alkoxy. The invention also discloses a preparation method of the polysubstituted 2-pyrrolopyridine derivative. The polysubstituted 2-pyrrolopyridine derivative shown in the formula is obtained at high yield after completing heating reaction of N-propargyl enaminone in a solvent in the presence of appropriate alkali. The polysubstituted 2-pyrrolopyridine derivative and the preparation method have the beneficial effects that the reaction conditions are mild; the reaction time is short; the range of substrates is wide; the reaction specificity is strong; the yield is high; aftertreatment is simple and convenient to carry out.
Owner:HUAQIAO UNIVERSITY

A kind of preparation method of trans tetrasubstituted olefin derivative

The invention discloses a preparation method of trans tetrasubstituted olefin derivatives, comprising the following steps: (1) adding alkali, alkyne, palladium catalyst, ligand, halogenated aromatic hydrocarbon, precursor compound and organic solvent into a reaction vessel , after filling repeatedly with nitrogen, react at 80-140°C for 12-36h; (2) dilute the material obtained in step (1) with ethyl acetate, and then wash with water to separate the organic phase; (3) the step ( 2) The obtained organic phase is dried, filtered, concentrated and subjected to column chromatography or thin layer chromatography to obtain the trans tetrasubstituted olefin derivative. The present invention can simultaneously obtain trans tetrasubstituted olefins substituted by tetraaryls and trans tetrasubstituted alkenes substituted by triaryls and trimethylsilicon, and has good regioselectivity, and can synthesize trans tetrasubstituted alkenes which are difficult to obtain by other methods compound.
Owner:HUAQIAO UNIVERSITY

2-(2-Aminobenzoyl)benzoic acid derivative and preparation method thereof

The invention discloses a preparation method of 2-(2-aminobenzoyl)benzoic acid derivative (formula 2), which comprises the compound represented by formula (1) in a solvent, in the presence of alkali, water and air to prepare The method of the present invention takes air oxygen as the oxygen source, and the raw materials used are cheap and easy to obtain, the yield is high, the atom is economical, the reaction specificity is strong, and the post-treatment is simple and green.
Owner:XIAMEN HUAXIA UNIV

Synthesis method of benzodioxyheterohexenone aromatic compounds

The invention provides a synthesis method of benzodioxyheterohexenone aromatic compounds, which comprises the following steps: halogenated alkane, salicylic acid or substituted salicylic acid and alkali into an organic solvent, reacting at 60-130 DEG C for 5-10 hours, and finally separating and purifying, wherein the halogenated alkane is dichloro- dibromo- or diiodo-alkane, and the mol ratio of the salicylic acid or substituted salicylic acid to the alkali is 1:(1-3). The method provided by the invention can solve the problems of narrow substrate range, rigid reaction conditions, long reaction time, multiple byproducts, low yield, need for strong acid, environment pollution and the like.
Owner:HUAQIAO UNIVERSITY
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