2486-70-6Relevant articles and documents
Novel preparation method of antihypertensive drug telmisartan intermediate
-
Paragraph 0074-0080, (2021/06/26)
The invention relates to an electric reduction preparation method of aminobenzoic acid represented by formula I and ester thereof. The preparation reaction of the method is shown in the description; and in the reaction formula, R is selected from hydrogen, a methyl group, an ethyl group, a benzyl group, a C3 or C4 straight-chain alkyl or branched-chain alkyl group, -NO2 is selected from 4-NO2 or 5-NO2, and Y is selected from H or 4-NHCOC3H7-n. The electroreduction preparation method of aminobenzoic acid and ester I thereof is characterized in that in a separated electrolytic cell, an acidic solution of nthe itrobenzoic acid and ester III thereof is taken as a catholyte; the voltage of a cathode working electrode relative to a reference electrode is 1.00-2.50 V; and an anolyte is an acidicsolution, the current density is 25.0-250.0 mA/cm, and the electrolysis temperature is 15-90 DEG C.
High Turnover Pd/C Catalyst for Nitro Group Reductions in Water. One-Pot Sequences and Syntheses of Pharmaceutical Intermediates
Gallou, Fabrice,Li, Xiaohan,Lipshutz, Bruce H.,Takale, Balaram S.,Thakore, Ruchita R.
supporting information, p. 8114 - 8118 (2021/10/25)
Commercially available Pd/C can be used as a catalyst for nitro group reductions with only 0.4 mol % Pd loading. The reaction can be performed using either silane as a transfer hydrogenating agent or simply a hydrogen balloon (μ1 atm pressure). With this technology, a series of nitro compounds was reduced to the desired amines in high chemical yields. Both the catalyst and surfactant were recycled several times without loss of reactivity.
Preparation method of benzimidazole compound
-
Paragraph 0029-0030, (2021/04/10)
The invention belongs to the field of pharmaceutical chemicals, and particularly relates to a preparation method of a benzimidazole compound. The benzimidazole compound is prepared by taking a halogenated benzoic acid amine compound as a reaction raw material through azidation reaction and cyclization reaction. The benzimidazole compound with high yield and high purity can be obtained, and the method is suitable for industrial production.
Synthetic method 2 - n-propyl -4 - methyl -6 - (1 -methylbenzimidazole -2 -yl) benzimidazole (by machine translation)
-
Paragraph 0029-0034; 0043-0046; 0055-0058; 0067-0070, (2020/10/04)
The invention relates to the technical field of synthesis of medical intermediates, and discloses a synthesis method of 2 - n-propyl -4 - methyl -6 - (1 -methylbenzimidazole -2 -yl) benzimidazole; S1: a condensation closed loop is obtained; and the reaction temperature is controlled to 3 - and the intermediate IV is N - [-4 - methyl -5 - (40 - 110 °C-methylbenzimidazole) 2 -nitrophenyl]-butylamide; S2: a reduction ring; and the preparation method comprises the following steps: S3: condensation ring-ring synthesis and intermediate IV of -4 -propyl -4 - 1 -6 - methyl 1 - S4 -2 - (-6 -methylbenzimidazol 2 -yl) benzimidazole -2 . 2 - N-propyl -4 - methyl -6 - (1 -methylbenzimidazole -2 -yl) benzimidazole is higher in purity, reduced in impurities and high in yield. (by machine translation)
Synthesis method of telmisartan intermediate 4-amino-3-methylbenzoic acid
-
, (2019/05/21)
The invention discloses a synthesis method of telmisartan intermediate 4-amino-3-methylbenzoic acid. According to the synthesis method, 2-methylaniline reacts with chloroformate under the action of acatalyst to obtain the 4-amino-3-methylbenzoic acid. The synthesis method has the advantages of few reaction step, easy availability of raw materials, few side reaction, high reaction yield, high product purity, low process cost, simple post-treatment operation, no pollution and no emission.
Preparation method of 3-methyl-4-aminobenzoic acid
-
Paragraph 0029-0059, (2017/08/30)
The invention provides a preparation method of 3-methyl-4-aminobenzoic acid and belongs to the technical field of chemical synthesis. According to the method, 3-methyl-4-nitrobenzoic acid and a quaternary ammonium salt type phase-transfer catalyst are added to a reaction device, a solvent is added, the mixture is stirred uniformly, reduced iron powder and protonic acid are added to react, and a reaction liquid is obtained; then the reaction device is cooled, sodium carbonate and activated carbon are added for decoloration, the PH value is adjusted to be alkaline, iron mud is filtered and washed twice with a sodium carbonate solution, a filtered stock and cleaning fluids are mixed, and a light yellow solution is obtained; acid is added to the light yellow solution until the PH value is adjusted to be slightly acid, off white precipitates are separated out, filtered, washed with water and dried, and 3-methyl-4-aminobenzoic acid is obtained. The preparation method is simple, low in cost and more suitable for industrial production, and the product yield reaches 90.1% at most.
Method for preparing 3-methyl-4-aminobenzoic acid through catalytic hydrogenation
-
Paragraph 0025-0047, (2018/01/12)
The invention provides a method for preparing 3-methyl-4-aminobenzoic acid through catalytic hydrogenation, belonging to the technical field of chemical synthesis. The method comprises the following steps: adding 3-methyl-4-nitrobenzoic acid and a solvent into a reaction vessel so as to obtain a 3-methyl-4-nitrobenzoic acid solution, and adjusting the pH value of the solution to be alkaline; pouring the obtained alkaline aqueous solution into an autoclave, adding a catalyst, respectively carrying out replacement with nitrogen and hydrogen for three times, introducing ammonia gas for 2 minutes, carrying out pressurizing with hydrogen to 3.45 MPa to 4.50 MPa, and carrying out a reaction under the pressure of 4.50 to 2.50 MPa at 100 to 160 DEG C so as to obtain a reaction solution; and subjecting the reaction solution to post-processing so as to obtain the 3-methyl-4-aminobenzoic acid. The method provided by the invention has the advantages of easily-available raw materials, simple operation, low production amount of three wastes, environmental friendliness, capability of reaching a mole yield up to 90%, and more applicability to industrial production.
One-pot synthesis of 1,4-disubstituted 1,2,3-triazoles from nitrobenzenes
Zhao, Fen,Chen, Zhen,Xie, Kai,Yang, Rui,Jiang, Yu-Bo
, p. 109 - 113 (2016/01/25)
A facile synthesis of 1,4-disubstituted 1,2,3-triazoles was achieved from nitrobenzenes and terminal alkynes under mild conditions. The reactions were successful for nitrobenzenes and terminal alkynes bearing various functionalities, from which the 1,2,3-triazole derivatives were smoothly synthesized through a four-step one-pot sequence.
HETEROCYCLIC COMPOUNDS FOR THE INHIBITION OF PASK
-
Paragraph 0175, (2014/05/24)
Disclosed herein are new heterocyclic compounds and compositions and their application as pharmaceuticals for the treatment of disease. Methods of inhibiting PAS Kinase (PASK) activity in a human or animal subject are also provided for the treatment of diseases such as diabetes mellitus.
One-pot palladium-catalyzed synthesis of selectively substituted phenanthridines by sequential aryl-aryl and heck couplings, aza-michael and retro-mannich reactions
Della Ca, Nicola,Motti, Elena,Mega, Antonio,Catellani, Marta
supporting information; experimental part, p. 1451 - 1454 (2010/08/19)
A catalytic synthesis of selectively substituted phenanthridines is achieved through a reaction sequence involving palladium/norbornene-catalyzed unsymmetrical aryl-aryl and Heck couplings followed by aza-Michael and retro-Mannich reactions. In spite of the many steps involved the method is very simple and allows the formation of selectively substituted phenanthridines under mild conditions in a straightforward one-pot reaction starting from readily available aryl iodides and bromides.
