- Preparation method of 3-aminopropanesulfonic acid
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The invention provides a synthesis method of 3-aminopropanesulfonic acid. The method comprises the following steps: carrying out sulfonation reaction on a 3-aminopropanol water solution and sulfur dioxide and/or sulfur trioxide under catalysis of a catalyst and a cocatalyst to obtain a 3-aminopropanesulfonic acid product in one step, adding an organic solvent into the reaction solution, and carrying out programmed cooling to promote crystallization of the 3-aminopropanesulfonic acid, and drying centrifugallyto obtain a qualified 3-aminopropanesulfonic acid product. The defects of high raw material toxicity and high energy consumption in the traditional preparation method are overcome.
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Paragraph 0037-0059
(2021/05/01)
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- Preparation method of nitrobenzoate
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The invention relates to the field of pesticides, and particularly discloses a preparation method of nitrobenzoate, wherein the structure of the nitrobenzoate is represented by a formula (2). The preparation method of the nitrobenzoate comprises the step that in the presence of a halogenated hydrocarbon organic solvent, a compound with a structure represented by the formula (1) makes contact withfuming nitric acid, fuming sulfuric acid and acetic anhydride, wherein in the formula (1) and the formula (2), X represents halogen, and R represents alkyl with the carbon atom number being 1-8. According to the method, the amount of waste acid can be reduced, and nitrobenzoate can be obtained at high yield.
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Paragraph 0041-0045; 0056; 0057
(2020/07/15)
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- Discovery of novel phenoxybenzamide analogues as Raf/HDAC dual inhibitors
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Histone deacetylase (HDAC)inhibitors as an important epigenetic therapeutic strategy affect signaling networks and act synergistically with kinase inhibitors for the treatment of cancer. Herein we presented a series of novel phenoxybenzamide analogues with inhibition of Raf and HDAC. Among them, compound 10e showed potent antiproliferative activities against Hepg2 and MDA-MB-468 in cellular assays. This work may lay the foundation for developing novel dual Raf/HDAC inhibitors as potential anticancer therapeutics.
- Geng, Aixin,Cui, Hao,Zhang, Liyuan,Chen, Xin,Li, Hongmei,Lu, Tao,Zhu, Yong
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supporting information
p. 1605 - 1608
(2019/05/02)
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- Tuning a robust system: N,O zinc guanidine catalysts for the ROP of lactide
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Non-toxic, highly active and robust complexes are the holy grail as ideal green catalysts for the polymerisation of biorenewable and biodegradable polylactide. Four new zinc guanidine complexes [ZnCl2(TMG4NMe2asme)], [ZnCl2(TMG5Clasme)], [ZnCl2(TMG5Measme)] and [ZnCl2(TMG5NMe2asme)] with different electron-donating and electron-withdrawing groups on the ligand's aromatic backbone have been synthesised. Ligands are derived from low-cost commercially available compounds and have been converted by a three- or four-step synthesis process into the desired ligand in good yields. The compounds have been fully characterised and tested in the ROP of rac-LA under industrially relevant conditions. The complexes are based on the recently published structure [ZnCl2(TMGasme)] which has shown high activity in the polymerisation of lactide at 150 °C. Different substituents in the para-position of the guanidine moiety significantly increase the polymerisation rate whereas positioning substituents in the meta-position causes no change in the reaction rate. With molecular weights over 71000 g mol-1 being achievable, the best system produces polymers for multiple industrial applications and its polymerisation rate approaches that of Sn(Oct)2. The robust systems are able to polymerise non-purified lactide. The initiation of the polymerisation is suggested to occur due to impurities in the monomer.
- Sch?fer, Pascal M.,McKeown, Paul,Fuchs, Martin,Rittinghaus, Ruth D.,Hermann, Alina,Henkel, Johanna,Seidel, Sebastian,Roitzheim, Christoph,Ksiazkiewicz, Agnieszka N.,Hoffmann, Alexander,Pich, Andrij,Jones, Matthew D.,Herres-Pawlis, Sonja
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p. 6071 - 6082
(2019/05/17)
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- PROCESS FOR PREPARING TOLVAPTAN INTERMEDIATES
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The present invention provides a novel process for the preparation of 7-chloro-2,3,4,5-tetrahydro-1H-1-benzazepin-5-one. The present invention also provides an improved process for the preparation of 7-chloro-1-(2-methyl-4-nitrobenzoyl)-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine. The present invention further provides an improved process for the preparation of 7-chloro-1-[2-methyl-4-[(2-methylbenzoyl)amino]benzoyl]-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine.
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Paragraph 0046; 0047
(2013/07/31)
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- Convenient synthesis of various substituted homotaurines from alk-2-enamides
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Various substituted homotaurines (=3-aminopropane-1-sulfonic acids) 6 were readily synthesized in satisfactory to good yields via the Michael addition of thioacetic acid to alk-2-enamides 3 (→4), followed by LiAlH4 reduction (→5) and performic acid oxidation (Scheme 1). The configuration of 'anti'-disubstituted homotaurine 'anti'-6h was deduced from the 3-(acetylthio)alkanamide (=S-(3-amino-1,2-dimethyl-3-oxopropyl) ethanethioate)'anti'-4h formed in the Michael addition, which was identified via the Karplus equation analysis, and confirmed by X-ray diffraction analysis. The current route is an efficient method to synthesize diverse substituted homotaurines, including 1-, 2-, and N-monosubstituted, as well as 1,2-, 1,N-, 2,N-, and N,N-disubstituted homotaurines (Table). Copyright
- Nai, Youfeng,Xu, Jiaxi
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p. 1355 - 1365
(2013/08/23)
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- PROCESS FOR PREPARING TOLVAPTAN INTERMEDIATES
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The present invention provides a novel process for the preparation of 7-chloro-2,3,4,5-tetrahydro-1H-1-benzazepin-5-one. The present invention also provides an improved process for the preparation of 7-chloro-1-(2-methyl-4-nitrobenzoyl)-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine. The present invention further provides an improved process for the preparation of 7-chloro-1-[2-methyl-4-[(2-methylbenzoyl)amino]benzoyl]-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine.
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Page/Page column 6
(2012/04/23)
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- Synthesis, characterization and evaluation of some 5-substituted 1,3,4-oxadiazole-2-thioesters as antifungal agents
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A series of 5-substituted 1,3,4-oxadiazole-2-thioesters was synthesized by converting several substituted organic acids successively into the corresponding esters, hydrazides and 5-substituted 1,3,4-oxadiazole-2-thiols. Finally the target compounds: 5-substituted 1,3,4-oxadiazole-2-thioesters were obtained by refluxing 5-substituted 1,3,4-oxadiazole-2-thiols in the presence of acid chloride and potassium hydroxide. The structures of the synthesized compounds were established by physicochemical and spectroscopic methods. The synthesized compounds were evaluated for their in vitro antifungal activity. Some of the evaluated compounds possessed significant antifungal activity as compared to a terbinafine standard.
- Hasan, Aurangzeb,Sheikh, Md Rezaul Karim,Gapil, Shelly
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experimental part
p. 2573 - 2578
(2012/09/07)
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- Synthesis of homotaurine and 1-substituted homotaurines from α,β-unsaturated nitriles
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Homotaurine and a series of 1-substituted homotaurines were readily synthesized in satisfactory to good yields via the Michael addition of thioacetic acid to aliphatic and aromatic α,β-unsaturated nitriles followed by lithium aluminum hydride mediated reduction and performic acid oxidation. The synthesis of 1,1-disubstituted homotaurines was attempted with β,β-disubstituted acrylonitriles as starting materials but failed due to steric hindrance. The current process is an efficient method for the synthesis of 1-substituted homotaurines. Georg Thieme Verlag Stuttgart New York.
- Ma, Yunhai,Xu, Jiaxi
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experimental part
p. 2225 - 2230
(2012/09/22)
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- Synthesis, characterization and antifungal activity of some new 5-substituted 1,3,4-oxadiazole-2-thiols
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A series of 5-substituted 1,3,4-oxadiazol-2-thiols (3a-i) was synthesized by refluxing variably substituted organic acids (Ra-i) with methanol to the corresponding esters (1a-i). These esters were then converted to hydrazides (2a-i) by reaction with hydrazine hydrate in the presence of absolute ethanol which was followed by reaction with carbon disulfide and potassium hydroxide. Structure of the synthesized compounds was established by physicochemical and spectral data analysis. Synthesized compounds were subjected to antifungal activity. Antifungal activity was performed against Aspergillus flavus, Mucor species, Aspergillus niger and Aspergillus fumigates, with test compounds at a concentration of 200 μg/mL. Terbinafine was used as the standard drug.
- Hasan, Aurangzeb,Gapil, Shelly,Khan, Izzat
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experimental part
p. 2007 - 2010
(2012/02/14)
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- Synthesis, characterization and antifungal activity of some 5-substituted 4-amino-1,2,4-triazole-3-thiols
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A series of 5-substituted 4-amino-1,2,4-triazole-3-thiols (4a-i) was synthesized by refluxing substituted organic acids (a-i) with methanol to the corresponding esters (1a-i). These esters were then converted to hydrazides (2a-i) by reaction with hydrazine hydrate in the presence of absolute ethanol. The hydrazides were then converted to 5-substituted 1,3,4-oxadiazole-2-thiols (3a-i) by cyclization reaction with carbon disulfide and KOH which was followed by reaction with hydrazine hydrate in the presence of absolute ethanol. Structure of the synthesized compounds was established by physico-chemical and spectral data analysis. Synthesized compounds were subjected to antifungal activity. Antifungal activity analysis was performed against Aspergillus flavus, Mucor species, Aspergillus niger and Aspergillus fumigates, with test compounds at a concentration of 200 μg/mL. Terbinafine was used as the standard drug.
- Hasan, Aurangzeb,Akhtar, Mohammad Nadeem,Gapil, Shelly
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scheme or table
p. 5471 - 5476
(2012/07/27)
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- HOMOGENEOUS TIME RESOLVED FLUORESCENCE BASED TEST SYSTEM
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The present invention concerns a fluorescence resonance energy transfer based high throughput test system to measure the formation of the HIV gp41 six-helix bundle. In a first embodiment the current invention relates to a homogeneous time resolved fluorescence-based test system comprising a first helical polypeptide consisting essentially of the sequence of IQN36 (SEQ ID NO:1); a second helical polypeptide consisting essentially of the sequence of C34 (SEQ ID NO: 2) wherein said IQN36 is labeled with a light emitting fluorophore and said C34 is labeled with an ultra-violet excitable fluorophore.
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Page/Page column 10
(2010/12/29)
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- BIS-ARYL COMPOUNDS FOR USE AS MEDICAMENTS
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There is provided compounds of formula I, wherein ring A, D1, D2a, D2b, D3, L1, Y1, L3 and Y3 have meanings given in the description, and pharmaceutically-acceptable salts thereof, which compounds are useful in the treatment of diseases in which inhibition of leukotriene C4 synthase is desired and/or required, and particularly in the treatment of a respiratory disorder and/or inflammation.
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Page/Page column 97
(2009/12/02)
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- Microwave-assisted esterification of diverse carboxylic acids and chiral amino acids
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A facile and efficient synthetic method of esters from their corresponding carboxylic acids and amino acids is described. The esterification reaction of carboxylic acids and amino acids could be greatly accelerated under microwave irradiation because the reactions described in this article took place in only 5 min with almost quantitative yields, and distinct acidity of catalytic acids was well tolerated. Unlike the racemation problem in microwave-assisted N-acylation reactions, the esters of chiral amino acids could be achieved with retention of configuration under this condition. Copyright Taylor & Francis Group, LLC.
- Yang, Qian,Wang, Xiao-Jian,Li, Zhi-Yu,Sun, Li,You, Qi-Dong
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experimental part
p. 4107 - 4115
(2009/04/04)
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- METHOD FOR MAKING BIARYL COMPOUNDS, COMPOUNDS MADE BY THE METHOD, AND METHOD FOR THEIR USE
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Certain disclosed embodiments of the present invention concern a method for making biaryl compounds by combining a diene with a dienophile under reaction conditions that facilitate a Diels-Alder reaction. Certain embodiments are particularly directed to making a tetra-ortho-substituted biaryl compounds. The disclosed method may involve using novel dienes, dienophiles, or both. Similarly, certain of the biaryl compounds are novel compounds too. Additional disclosed embodiments concern a method for making useful compounds by first making a Diels-Alder adduct. The Diels-Alder adduct is then further modified or coupled to other compounds. The method can be used to make carbazoles, such as Siamenol. Disclosed biaryl compounds are useful for a number of applications, such as pharmacophores and organocatalysts.
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Page/Page column 44; 179-180
(2009/01/23)
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- Diels - Alder approach for the construction of halogenated, o-nitro biaryl templates and application to the total synthesis of the anti-HIV agent siamenol
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(Chemical Equation Presented) A rapid Diels - Alder approach to halogenated biaryl templates is described. These biaryl templates are available in two steps from the corresponding aromatic aldehydes. The scope of subsequent Suzuki couplings on the biaryl chlorides is explored. Good tolerance for both electron-donating and electron-withdrawing groups in the coupling process can be achieved. Further functionalization of the biaryl templates is described. Hydrogenation of the nitro moiety with concomitant removal of the benzyl ether yields the o-anilino, o-phenolic polyaryls. Selective reduction of the nitro group can be accomplished. Alternatively, the benzyl ether can be selectively removed under Lewis acidic conditions. The utilization of the Diels - Alder adducts for the synthesis of a series of chlorinated carbazoles via the Cadogan cyclization is also demonstrated. Finally, application of this technology to the total synthesis of siamenol, an anti-HIV agent, is reported.
- Naffziger, Michael R.,Ashburn, Bradley O.,Perkins, Johanna R.,Carter, Rich G.
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p. 9857 - 9865
(2008/04/05)
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- COMPOUND INHIBITING IN VIVO PHOSPHORUS TRANSPORT AND MEDICINE CONTAINING THE SAME
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An objective of the present invention is to provide compounds that can effectively suppress the concentration of phosphorus in serum to effectively prevent or treat diseases induced by an increase in concentration of phosphate in serum. The compounds according to the present invention are compounds represented by formula (I) and pharmaceutically acceptable salts and solvates thereof: wherein A represents an optionally substituted five- to nine-membered unsaturated carbocyclic moiety or a five- to nine-membered unsaturated heterocyclic moiety, and ---- represents a single bond or a double bond, R5 represents optionally substituted aryl or the like, Z represents - N=CHR6R7 or the like, R6 and R7 represent H, optionally substituted alkyl, optionally substituted aryl or the like, R101 and R102 together form =O, and R103 and R104 represent H, or R101 and R104 together from a bond, and R102 and R103 together form a bond.
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Page/Page column 161
(2010/11/08)
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- Relative reactivity of methyl iodide to ethyl iodide in nucleophilic substitution reactions in acetonitrile and partial desolvation accompanying activation
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Through the examination of empirical correlations involving activation parameters for nucleophilic substitution of methyl iodide and of ethyl iodide, nucleophiles have been classified into three series: (1) nucleophiles with two equivalent reaction sites, (2) nucleophiles with a chlorine atom in the para-position, and (3) nucleophiles with a single reaction site. Three types of partial desolvation processes accompanying activation have been deduced on the basis of these classifications. A major factor determining the relative reactivity of methyl iodide to ethyl iodide in the substitution reaction of an anionic nucleophile having a single reaction site in acetonitrile (kMeI/kEtI) is suggested to be partial desolvation around the nucleophilic center on going from reactant to transition-state.
- Kondo, Yasuhiko,Urade, Miyuki,Yamanishi, Yukari,Chen, Xinyu
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p. 1449 - 1454
(2007/10/03)
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- 7-Chloro-5-hydroxy-1-[2-methyl-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5- tetrahydro-1H-1-benzazepine (OPC-41061): A potent, orally active nonpeptide arginine vasopressin V2 receptor antagonist
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We previously reported a series of benzazepine derivatives as orally active nonpeptide arginine vasopressin (AVP) V2 receptor antagonists. After the lead structure OPC-31260 was structurally evaluated and optimized, the introduction of the 7-Cl moiety on the benzazepine and 2-CH3 on the aminobenzoyl moiety enhanced its oral activity. The new AVP-V2 selective antagonist OPC-41061 was determined to be a potent and orally active agent. Copyright (C) 1999 Elsevier Science Ltd.
- Kondo, Kazumi,Ogawa, Hidenori,Yamashita, Hiroshi,Miyamoto, Hisashi,Tanaka, Michinori,Nakaya, Kenji,Kitano, Kazuyoshi,Yamamura, Yoshitaka,Nakamura, Shigeki,Onogawa, Toshiyuki,Mori, Toyoki,Tominaga, Michiaki
-
p. 1743 - 1754
(2007/10/03)
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- A study of 3-amino-N-hydroxypropanesulfonamide derivatives as potential GABA(B) agonists and their fragmentation to 3-aminopropanesulfinic acid
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A series of 3-amino-N-hydroxypropanesulfonamide analogs were prepared. Several compounds showed potent binding at the GABA(B) receptor and were active in an in vitro functional assay. The GABA(B) activity of these compounds appeared to be due to the fragmented product, 3-aminopropanesulfinic acid.
- Shue, Ho-Jane,Chen, Xiao,Blythin, David J.,Carruthers, Nicholas I.,Spitler, James M.,Wong, Shing-Chun,Chapman, Richard W.,Rizzo, Charles,West, Robert,She, Hoyan S.
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p. 1709 - 1714
(2007/10/03)
-
- QUINAZOLINONE AND PYRIDOPYRIMIDINE A-II ANTAGONISTS
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Substituted quinazolinones and pyridopyrimidines of structural formula 1 STR1 are angiotensin II antagonists useful in the treatment of disorders related to the reninangiotensin system (RAS) such as hypertension, congestive heart failure, ocular hypertension and certain CNS disorders.
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-
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- QUINAZOLINONES AND PYRIDOPYRIMIDINONES
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Substituted quinazolinones and pyridopyrimidines of structural formula I STR1 are angiotensin II antagonists useful in the treatment of disorders related to the renin-angiotensin system (RAS) such as hypertension, congestive heart failure, ocular hypertension and certain CNS disorders.
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- Preparation of trifluoromethylphenyl nitrophenylethers
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A process for preparing trifluoromethylphenyl nitro phenylethers which comprises treating a trifluoromethylhalobenzene with a base in a cosolvent system to afford a trifluoromethyl phenolate which may be isolated as its free phenol or reacted with an appropriately substituted halobenzene to afford a diphenylether herbicide or a precursor thereto.
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- Hydroxypropylene-amino-phosphonic-sulfonic acids
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This invention relates to compounds characterized by the presence of N-methyl, or substituted methyl, phosphonic acid and N-hydroxy-propylenesulfonic acid groups. These compounds contain at least one or more of each group and are bonded to the same or different amino groups. They are derived by reacting an amine with both (1) an epihalohydrin-bisulfite addition product and (2) with a carbonyl compound, such as formaldehyde, and phosphorous acid or its equivalent. They have a wide variety of uses, for example as scale and corrosion inhibitors, iron oxide removers, chelating agents, etc.
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- Probiotics. Antistaphylococcal and antifibrinolytic activities of omega amino and omega guanidinoalkanesulfonic acids
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A series of ;. aminoalkanesulfonic acid and ω guanidinoalkanesulfonic acids was tested for antistaphylococcal and antifibrinolytic activities. Most of the former and one of the latter class gave better protection against Staphylococcus aureus infections in mice than 4 aminobutyryl L histidine. Most of the ω aminoalkanesulfonic acids showed antifibrinolytic activity, one of them having activity equal to or greater than that of aminocaproic acid, whereas none of the ω guanidinoalkanesulfonic acids had significant antifibrinolytic activity.
- Fujii,Cook
-
p. 502 - 505
(2007/10/05)
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