19results about How to "Short reaction steps" patented technology

The invention discloses a synthesis method of a 2 '-(trifluoromethyl)-4, 5-dihydro-spiro [furan-2, 3'-indoline] derivative, and belongs to the technical field of organic synthesis.The 2 '-(trifluoromethyl)-4, 5-dihydro-spiro [furan-2, 3'-indoline] derivative is obtained by synthesizing 2 '-(trifluoromethyl)-4, 5-dihydro-spiro [furan-2, 3'-indoline] in the presence of visible light, a photocatalyst and alkali. CF3Br and a 3-(3-hydroxypropyl) indole derivative are subjected to a free radical tandem cyclization reaction in an organic solvent to prepare the 3-(3-hydroxypropyl) indole derivative. According to the 2 '-(trifluoromethyl)-4, 5-dihydro-spiro [furan-2, 3'-indoline] derivative and the preparation method thereof, CF3Br is used as a trifluoromethyl source under photocatalysis for the first time, trifluoromethyl is directly introduced into an indoline ring of 4, 5-dihydro-spiro [furan-2, 3 '-indoline], the 2'-(trifluoromethyl)-4, 5-dihydro-spiro [furan-2, 3 '-indoline] derivative is obtained, and the compound has good activity and selectivity on cancer cells such as Huh-7, A549 and A549 / DDP.

The invention discloses a synthesis method of 4-amino-N-tert-butylbenzamide, which comprises the following steps: by taking p-aminobenzonitrile and tert-butyl acetate as initial raw materials, carrying out Ritter reaction in an acidic system to prepare the 4-amino-N-tert-butylbenzamide in one step; the acidic system is composed of an acidic solvent and an acidic catalyst; the acidic solvent is acetic acid; the acid catalyst is p-toluenesulfonic acid or sulfuric acid. The method provided by the invention not only solves the problem that the tert-butylamine and other raw materials with pungent smell need to be adopted in the prior art and are not friendly to human bodies and environment, but also avoids the problems of low safety caused by a high-risk process and high production cost caused by the need of adopting an expensive palladium catalyst in the prior art; particularly, the method is short in reaction step, simpler and more convenient to operate, more stable in process and suitable for large-scale industrial production.

The present invention proposes a dihydropyrroloquinazolinone compound containing trifluoromethyl and a synthesis method thereof, and belongs to the technical field of organic synthesis. The dihydropyrroloquinazolinone compound containing trifluoromethyl of the present invention is prepared by a free radical tandem cyclization reaction of CF3Br and N-cyano-N-alkenylamide in an organic solvent under visible light induction and the presence of a photocatalyst and a base. The present invention is the first to regulate the regioselectivity of the substrate under photocatalysis, directly introduce the trifluoromethyl group into the dihydropyrroloquinazolinone ring, and obtain a trifluoromethyl-substituted dihydropyrroloquinazolinone, which can be further used to prepare drugs with anti-Alzheimer's disease. The present invention provides a new method for the synthesis of functionalized dihydropyrroloquinazolinone compounds, which has the advantages of cheap and readily available raw materials, short reaction steps, high regioselectivity of the reaction, simple operation, mild reaction conditions, and good reaction yield.

In the presence of an acidic reagent and an oxidizing agent, 2-indolone and indole are used as raw materials for one-step reaction to prepare the symmetric and asymmetric indole [2, 3-a] carbazole derivatives, the used raw materials, the acidic reagent and the oxidizing agent are cheap and easy to obtain, the reaction system is simple, the operation is simple, and the reaction steps are short (one-step reaction); the method has the advantages of wide substrate applicability, good functional group compatibility, mild reaction conditions, fast reaction speed, good chemical selectivity, realization of industrial production, and substantial economic and social benefits.

The invention discloses a method for preparing 2,4,5-trifluorophenylacetic acid, and relates to the technical field of organic chemical industry. Aluminum chloride is added to 1,2,4-trifluorobenzene, methyl bromide is introduced under stirring to react, a solvent and sodium hydrogen are continuously added to the obtained 2,4,5-trifluorotoluene, carbon dioxide is continuously introduced, and reacted at 25-35 DEG C to obtain 2,4,5-trifluorophenylacetic acid sodium, filtered, quenched, and then adjusted to pH below 2 with 30%wt hydrochloric acid, and 2,4,5-trifluorophenylacetic acid solid is obtained by filtration. The whole reaction process is simple to operate, the reaction conditions are mild, the environmental pollution is small, it is suitable for industrial production, and the yield and purity of the product are high.

The invention discloses a method for efficiently preparing a teniposide precursor, which comprises the following steps of: protecting 4 '-demethyl epipodophyllotoxin serving as an initial material by phenol to generate an intermediate I; secondly, alpha-anhydrous glucose ester is used as a substrate, selective protection of hydroxyl is carried out, and an intermediate II is generated; then, under the catalysis of BF3. Et2O, the intermediate I and the intermediate II are coupled to generate an intermediate III; finally, through hydrogenolysis, an intermediate IV can be prepared, and the intermediate IV is used as a key precursor for synthesizing teniposide. According to the scheme, a more efficient sugar ring building block (intermediate II) is selected, so that the reaction efficiency can be improved, and excellent selectivity is achieved. The route has the advantages of short reaction steps (only four steps) and high yield, and solves the problem of later deacetylation of the coupled sugar ring building block, thereby greatly reducing the unit cost.

This invention relates to the field of compound synthesis technology, specifically disclosing a method for preparing 8-chloronaphtho[1,2-b]benzofuran. The preparation method includes the following steps: mixing compound 1 with a solvent, then adding sodium hydroxide and sodium chloride, followed by dropwise addition of an aqueous solution of sodium hypochlorite, stirring the reaction mixture to obtain the target compound 8-chloronaphtho[1,2-b]benzofuran. The preparation method provided by this invention is low-cost and has a high yield.

The invention develops a methodological strategy for rapidly constructing a 3-oxazoline-5-ketone skeleton by taking an amino acid derivative and an imine ketone ester as substrates to obtain a compound containing 3-oxazoline-5-ketone substituted allene. The synthesis of the oxazolinone substituted allene compound with potential important biological activity and application value is realized. The oxazolinone is simple in structure, easy to prepare, wide in derivation range and low in price, and the structural diversity of oxazolinone compounds can be better enriched. The method disclosed by the invention can be prepared by a one-pot method, is efficient and rapid, simple to operate, short in reaction step, mild in reaction condition and wide in application range, and overcomes the defects of complex operation, harsh reaction condition, limited substrate, intolerant substrate functional groups, tedious steps and the like of the traditional reaction.

The invention discloses a preparation method of p-phenylene-bis-benzene trimellitate dianhydride, and relates to the technical field of preparation of organic compounds. The preparation method provided by the invention comprises the following steps: mixing chlorinated trimellitic anhydride, hydroquinone and a catalyst, and reacting to obtain a p-phenylene-bis-benzene trimellitate dianhydride crude product; and recrystallizing the p-phenylene-bis (trimellitate) dianhydride crude product, mixing with acetic anhydride, and reacting to obtain the p-phenylene-bis (trimellitate) dianhydride, the catalyst is prepared from at least one of pyridine, triethylamine, N, N-diisopropylethylamine, diethylamine and dimethylamine. The preparation method provided by the invention improves the purity and whiteness of p-phenylene-bis (trimellitate) dianhydride, and has the advantages of short reaction steps, mild conditions, simple post-treatment, high yield, simple refining steps, high product purity and the like.

The invention relates to a method for preparing an indacaterol intermediate 5,6-diethyl-2,3-dihydro-1H-inden-2-amine hydrochloride, comprising the following steps: 1,3-dihydro-2H-inden-2-one and hydroxylamine hydrochloride are subjected to an oximation reaction to obtain 1,3-dihydro-2H-inden-2-ketone oxime; 1,3-dihydro-2H-inden-2-ketone oxime is subjected to a bromination reaction to obtain 5,6-dibromo-1,3-dihydro-2H-inden- 2-ketoxime; 5,6-dibromo-1,3-dihydro-2H-indene-2-ketoxime and vinyl n-butyl ether are subjected to Heck reaction and then hydrolyzed to obtain 5,6-diacetyl-1,3-dihydro-2H-indene-2-ketoxime; 5,6-diacetyl-1,3-dihydro-2H-indene-2-ketoxime is subjected to hydrogenation reaction and then salted to obtain the target product 5,6-diethyl-2,3-dihydro-1H-indene-2-amine hydrochloride. The invention is easy to scale up industrially and has low cost.

The invention provides a method for preparing 9,9-bis(3,4-dicarboxyphenyl)fluorene anhydride, comprising the following steps: S1: mixing fluorene, phthalic anhydride, an inorganic salt and a solvent to obtain a mixed solution A; S2: heating the mixed solution to a certain temperature, reacting for a period of time, cooling, filtering, treating the filtrate, and precipitating 9,9-bis(3,4-dicarboxyphenyl)fluorene anhydride. The method for preparing 9,9-bis(3,4-dicarboxyphenyl)fluorene anhydride of the present invention has the advantages of short reaction steps, easy purchase of raw materials and low cost, simple post-processing operation, high yield, high product purity and less environmental pollution.

The invention discloses a method for preparing 2,5-dimethylphenylacetic acid, and belongs to the technical field of fine chemicals. 2,5-dimethylbenzoyl chloride is used as a raw material, reacts with sodium cyanide in an acetonitrile solution to obtain 2,5-dimethylbenzoyl nitrile; then 2,5-dimethylbenzoyl nitrile is subjected to a reduction hydrolysis reaction with hydrazine hydrate and potassium hydroxide in a 1,3-propylene glycol solution, and 2,5-dimethylphenylacetic acid is obtained by acidification and filtration. The method has short reaction steps, simple operation, mild reaction conditions, high yield and product purity, and is very easy to realize industrial production.

This invention discloses a method for preparing cefotaxime derivatives, comprising the following steps: (1) hydroxyl protection; (2) reduction / substitution: the reduction step is: the obtained 2,3-di(methoxymethoxy)benzaldehyde reacts with sodium borohydride to obtain the corresponding 2,3-di(methoxymethoxy)benzyl alcohol (intermediate 2); or the substitution step is: the obtained 2,3-di(methoxymethoxy)benzaldehyde reacts with RMgBr to obtain the hydroxyl carbon-substituted product of 2,3-di(methoxymethoxy)benzyl alcohol (intermediate 2). (3) Mitsunobu reaction; (4) hydrazinolysis; (5) condensation; (6) amidation; (7) deprotection; (8) deprotection to obtain cefotaxime derivatives. The process is simple and can synthesize a variety of cefotaxime derivatives.

The application relates to the technical field of compound synthesis, and particularly discloses a preparation method of 2-bromofluorenone. According to the method, 4-bromo-2'-iodo-biphenyl is reacted with carbon dioxide under the action of a strong base to generate 2-bromofluorenone in one step, the reaction step is short, the production cost is greatly reduced, the reaction condition is mild, the process operation is simple, the post-treatment of the reaction is simple, the product with high purity can be easily obtained, and the method is suitable for process amplification production.

The application discloses a method for preparing heliotropin, which comprises the following steps: taking piperine as a raw material, and performing chloromethylation and oxidation reaction to obtain heliotropin, wherein water is used as a solvent in the oxidation step, and oxygen-containing gas is used as an oxidant; the reaction is performed under normal pressure, the conditions are mild, the three wastes are less, the selectivity is good, and the yield is high, so the method is a better industrial production method.

The invention belongs to the field of medicine preparation, and particularly relates to a preparation method of oleanolic acid ester glycoside. The preparation method comprises the following steps: reacting oleanolic acid with monosaccharide under the action of dicyclohexylcarbodiimide and 4-dimethylaminopyridine; extracting reactants to obtain a crude product; and recrystallizing the crude product. The oleanolic acid ester glycoside prepared by adopting the synthesis method disclosed by the invention is relatively high in yield and purity, short in reaction step, low in cost, simple in post-treatment and suitable for industrial production, and has a good application prospect.

The invention provides a method for synthesizing bicyclol, and belongs to the field of medicine synthesis. The invention provides a method for synthesizing bicyclol, which comprises the following steps: by taking biphenyl alcohol acid as an initial raw material, adding methyl tert-butyl ether and a catalyst for reaction, and purifying, thereby obtaining the bicyclol. The catalyst is iron trifluoromethanesulfonate; the synthetic route of the compound is # imgabs0 #. According to the method for synthesizing the bicyclol, provided by the invention, a new methylation reagent methyl tert-butyl ether and a catalyst iron trifluoromethanesulfonate are adopted, and methylation reagents which are high in toxicity, easy to explode and the like and are extremely easy to generate dangers in the use process are avoided, so that the defects of harsh post-treatment, poor reaction selectivity, low yield and the like in the existing process are overcome; the method has the advantages of short reaction steps, simple process operation, mild conditions, high yield, safe and reliable product quality, stable process and good reproducibility; the materials in the whole process are cheap, easy to obtain and non-toxic, the used materials and the operation process are friendly to EHS, and the method is suitable for industrial production.

The invention provides a synthesis method of iodobenzonitrile octanoate, which comprises the following steps: step 1, iodination reaction: in water, mixing p-cyanophenol, an iodination reagent, an acid solution and a catalyst to carry out reaction I, and then dropwise adding hydrogen peroxide to carry out reaction II to obtain 3, 5-diiodine-4-hydroxybenzonitrile; step 2, esterification reaction: dropwise adding an acid-binding agent and capryloyl chloride into a mixed solution of 3, 5-diiodine-4-hydroxybenzonitrile and a solvent, and carrying out reaction III to obtain capryloyl iodobenzonitrile; in the synthesis method, water is used as a reaction solvent during iodination reaction, so that the use of an organic solvent is avoided, the use of the organic solvent is reduced, the synthesis method is environment-friendly, the cost is reduced, a reaction system is mild, and industrial production is easy to realize; in the esterification reaction, an industrial common aromatic solvent benzene is used, is easy to recover and remove water, and can be recycled through simple water washing, liquid separation and water treatment.

The invention discloses a method for preparing cyflumetofen, which comprises the steps of (1) reacting raw materials p-tert-butylphenylacetonitrile and bis(2-methoxyethyl) carbonate in an aprotic solvent in the presence of an alkaline substance to obtain 2-(4-tert-butylphenyl)-2-cyanoacetic acid (2-methoxy) ethyl ester; and (2) reacting the 2-(4-tert-butylphenyl)-2-cyanoacetic acid (2-methoxy) ethyl ester obtained in the step (1) with o-trifluoromethylbenzoyl chloride in the presence of an alkaline substance to obtain cyflumetofen. The method for preparing cyflumetofen of the invention has short reaction steps, mild reaction conditions, high yield and total yield of the reaction for synthesizing 2-(4-tert-butylphenyl)-2-cyanoacetic acid (2-methoxy) ethyl ester, and high product purity, easy to obtain raw materials, simple reaction operation and post-treatment, low environmental pollution, and is suitable for industrial production.