- Efficient and recyclable bimetallic Co–Cu catalysts for selective hydrogenation of halogenated nitroarenes
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Silica supported N-doped carbon layers encapsulating Co–Cu nanoparticles (Co1Cux@CN/SiO2) were prepared by a one-step impregnation of Co(NO3)2·6H2O, Cu(NO3)2·3H2O, urea and glucose, following in situ carbothermal reduction. Effects of Cu contents on the catalytic performance of the Co1Cux@CN/SiO2 catalysts were investigated for selective hydrogenation of p-chloronitrobenzene to p-chloroaniline. The Co1Cu0.30@CN/SiO2 with Cu/Co molar ratio of 0.30:1 presented much higher activity and stability than the monometallic Co@CN/SiO2 catalyst. The addition of Cu into Co1Cux@CN/SiO2 catalysts had favorable effects on the formation of highly active Co–N sites and N-doped carbon layer. The role of the N-doped carbon layer was to protect the Co from oxidation by air, and the Co1Cu0.30@CN/SiO2 could be reused for at least 12 cycles without decrease in catalytic efficiency. Mechanistic and in situ infrared studies revealed that the interaction effect between the Co and Cu atoms made the surface of Co highly electron rich, which decreased adsorption of halogen groups and resulting in the enhanced selectivity during chemoselective hydrogenation of halogenated nitroarenes for a wide scope of substrates.
- Lu, Xionggang,Ren, Jiaan,Sheng, Yao,Wang, Xueguang,Wu, Baoqin,Zou, Xiujing
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- Activator free, expeditious and eco-friendly chlorination of activated arenes by N-chloro-N-(phenylsulfonyl)benzene sulfonamide (NCBSI)
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N-Chloro-N-(phenylsulfonyl)benzene sulfonamide (NCBSI) has been explored for the first time as a chlorinating reagent for direct chlorination of various activated arenes and heterocycles without any activator. A comparative in-silico study was performed to determine the electrophilic character for NCBSI and commercially available N-chloro reagents to reveal the reactivity on a theoretical viewpoint. The reagent was prepared by an improved method avoiding the use of hazardous t-butyl hypochlorite. This reagent was proved to be very reactive compared to other N-chloro reagents. The precursor of the reagent N-(phenylsulfonyl)benzene sulfonamide was recovered from aqueous spent, which can be recycled to synthesize NCBSI. The eco-friendly protocol was equally applicable for the synthesis of industrially important chloroxylenol as an antibacterial agent.
- Misal, Balu,Palav, Amey,Ganwir, Prerna,Chaturbhuj, Ganesh
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supporting information
(2021/01/04)
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- In Situ Synthesized Silica-Supported Co@N-Doped Carbon as Highly Efficient and Reusable Catalysts for Selective Reduction of Halogenated Nitroaromatics
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Silica-supported Co@N-doped carbon (Co@CN/SiO2) catalysts were first prepared by a one-step impregnation with a mixed solution of cobalt nitrate, glucose and urea, followed by in situ carbonization and reduction. The Co@CN/SiO2 catalysts were investigated for the selective reduction of nitro aromatics to the corresponding anilines using hydrazine hydrate. The Co@CN/SiO2-500 carbonized at 500 °C exhibited the highest catalytic activity and excellent stability without any decay of activity after 6 cycles for the reduction of nitrobenzene. Both metallic Co atoms and Co?N species formed in the Co@CN/SiO2 catalysts were active, but the Co?N species were dominant active sites. The high activities of the Co@CN/SiO2 catalysts were attributed to the synergistic effect between the Co and N atoms, promoting heterolytic cleavage of hydrazine to form H+/H? pairs. Representative examples demonstrated that the Co@CN/SiO2-500 could completely transform various halogen-substituted nitro aromatics to the corresponding halogenated anilines with high TOFs and selectivity of '99.5 percent.
- Sheng, Yao,Wang, Xueguang,Yue, Shengnan,Cheng, Gonglin,Zou, Xiujing,Lu, Xionggang
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p. 4632 - 4641
(2020/07/30)
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- Highly selective hydrogenation of halogenated nitroarenes over Ru/CN nanocomposites by: In situ pyrolysis
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A highly chemoselective and recyclable ruthenium catalyst for the hydrogenation of halogenated nitroarenes has been prepared via the simple in situ calcination of a mixture of melamine, glucose and ruthenium trichloride. Superfine Ru particles (2.3 ± 0.3 nm) were obtained and highly dispersed in the nitrogen-doped carbon matrix. The Ru/CN catalyst smoothly transforms a variety of halogenated nitroarenes to the corresponding haloanilines with high intrinsic activity (e.g. TOF = 1333 h-1 for p-chloronitrobenzene) and selectivity of more than 99.6percent. Furthermore, through an analysis of the products in the reaction process, it was concluded that there are two parallel reaction pathways (a direct pathway and an indirect pathway) for the hydrogenation of aromatic nitro compounds over the Ru/CN catalyst, and the direct pathway was proved to be dominant in catalyzing the intermediates. This journal is
- Yue, Shengnan,Wang, Xueguang,Li, Shaoting,Sheng, Yao,Zou, Xiujing,Lu, Xionggang,Zhang, Chunlei
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p. 11861 - 11869
(2020/07/28)
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- Process study for synthesizing 2,3,6-trichloropyridine from nicotinamide
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The invention provides a process study for synthesizing 2,3,6-trichloropyridine from nicotinamide. The process study comprises the following steps: with nicotinamide as a raw material, adding a sodiumhypochlorite solution in an alkaline environment to carry out a Hofmann downgrading reaction to obtain 3-aminopyridine; under catalysis of a Lewis acid catalyst, performing chlorination reaction under a concentrated hydrochloric acid/hydrogen peroxide condition to obtain 2,6-dichloro-3-aminopyridine; and reacting in the presence of sodium nitrite under low temperature and strong acid conditions to form a diazonium salt solution; and finally, performing a Sandmeyer reaction to obtain the target product, 2,3,6-trichloropyridine. The process material provided by the invention is simple, easily available and cheap, the reaction condition is simple and easy to operate, the post-treatment is simple, the yield is high, and thus the process has good industrial development prospects.
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- INHIBITORS OF SHORT-CHAIN DEHYDROGENASE ACTIVITY FOR PROMOTING NEUROGENESIS AND INHIBITING NERVE CELL DEATH
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A method of promoting neuroprotection in a subject from axonal degeneration, neuronal cell death, and/or glia cell damage after injury, augmenting neuronal signaling underlying learning and memory, stimulating neuronal regeneration after injury, and/or treating a disease, disorder, and/or condition of the nervous system in a subject in need thereof includes administering to the subject a therapeutically effective amount of a 15-PGDH inhibitor.
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Paragraph 00247
(2018/02/27)
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- ANTAGONISTS OF PROSTAGLANDIN EP3 RECEPTOR
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Provided herein are antagonists la or lb of prostaglandin EP3 receptor, processes to make said antagonists, and methods comprising administering said antagonists to a mammal in need thereof. (Formula I)
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Page/Page column 47
(2016/07/27)
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- Metal-Free Reduction of Aromatic Nitro Compounds to Aromatic Amines with B2pin2 in Isopropanol
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A metal-free reduction of aromatic nitro compounds to the corresponding amines has been achieved by a combination of B2pin2 and KOtBu in isopropanol. A series of nitro compounds containing various reducible functional groups were chemoselectively reduced in good to excellent yields.
- Lu, Hongtao,Geng, Zhiyue,Li, Jingya,Zou, Dapeng,Wu, Yusheng,Wu, Yangjie
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supporting information
p. 2774 - 2776
(2016/06/15)
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- INHIBITORS OF SHORT-CHAIN DEHYDROGENASE ACTIVITY FOR TREATING FIBROSIS
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A method of treating or preventing a fibrotic disease, disorder or condition includes administering to a subject in need of treatment a 15-PGDH inhibitor.
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Paragraph 00258
(2016/09/26)
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- Story of an Age-Old Reagent: An Electrophilic Chlorination of Arenes and Heterocycles by 1-Chloro-1,2-benziodoxol-3-one
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By the use of 1-chloro-1,2-benziodoxol-3-one, an age-old reagent, the practical and efficient chlorination method is achieved. This hypervalent iodine reagent is amenable not only to the chlorination of nitrogen-containing heterocycles but also to selected classes of arenes, BODIPY dyes, and pharmaceuticals. In addition, the advantages, such as easy preparation and recyclable, air- and moisture-stable, in combination with the success in a gram-scale experiment grant this reagent great potential for industrial application.
- Wang, Mengzhou,Zhang, Yanyan,Wang, Tao,Wang, Chao,Xue, Dong,Xiao, Jianliang
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supporting information
p. 1976 - 1979
(2016/06/01)
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- COMPOSITIONS AND METHODS OF MODULATING SHORT-CHAIN DEHYDROGENASE ACTIVITY
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Compounds and methods of modulating 15-PGDH activity, modulating tissue prostaglandin levels, treating disease, diseases disorders, or conditions in which it is desired to modulate 15-PGDH activity and/or prostaglandin levels include 15-PGDH inhibitors described herein.
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Paragraph 00452
(2015/05/19)
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- 7-HYDROXY-SPIROPIPIPERIDINE INDOLINYL ANTAGONISTS OF P2Y1 RECEPTOR
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The present invention provides compounds of Formula (I): as defined in the specification and compositions comprising any of such novel compounds. These compounds are antagonists of Ρ2Y1 receptor and may be used as medicaments in the treatment and/or prophylaxis of thromboembolic disorders.
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Paragraph 00221-00222
(2014/02/16)
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- Selective catalytic hydrogenation of nitro groups in the presence of activated heteroaryl halides
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Chemoselective reduction of nitro groups in the presence of activated heteroaryl halides was achieved via catalytic hydrogenation with a commercially available sulfided platinum catalyst. The optimized conditions employ low temperature, pressure, and catalyst loading (0.1 mol % Pt) to afford heteroaromatic amines with minimal hydrodehalogenation byproducts.
- Kasparian, Annie J.,Savarin, Cecile,Allgeier, Alan M.,Walker, Shawn D.
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experimental part
p. 9841 - 9844
(2012/01/06)
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- Dipyridodiazepinone derivatives; synthesis and anti HIV-1 activity
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Ten dipyridodiazepinone derivatives were synthesized and evaluated for their anti HIV-1 reverse transcriptase activity against wildtype and mutant type enzymes, K103N and Y181C. Two of them were found to be promising inhibitors for HIV-1 RT.
- Khunnawutmanotham, Nisachon,Chimnoi, Nitirat,Techasakul, Supanna,Thitithanyanont, Arunee,Saparpakorn, Patchreenart,Hannongbua, Supa,Choowongkomon, Kiattawee,Pungpo, Pornpan
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supporting information; experimental part
(2010/04/22)
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- Novel 2-chloro-8-arylthiomethyldipyridodiazepinone derivatives with activity against HIV-1 reverse transcriptase
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Based on the molecular modeling analysis against Y181C HIV-1 RT, dipyridodiazepinone derivatives containing an unsubstituted lactam nitrogen and 2-chloro-8-arylthiomethyl were synthesized via an efficient route. Some of them were evaluated for their antiviral activity against HIV-1 RT subtype E and were found to exhibit virustatic activity comparable to some clinically used therapeutic agents.
- Khunnawutmanotham, Nisachon,Chimnoi, Nitirat,Saparpakorn, Patchareenart,Pungpo, Pornpan,Louisirirotchanakul, Suda,Hannongbua, Supa,Techasakul, Supanna
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p. 218 - 230
(2007/10/03)
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- PROCESS FOR THE MANUFACTURE OF 2,3-DICHLOROPYRIDINE
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A method for preparing 2,3-dichloropyridine is disclosed in which 3-amino-2-chloropyridine is contacted with an alkali metal nitrite in the presence of aqueous hydrochloric acid to form a diazonium salt; and the diazonium salt is subsequently decomposed in the presence of copper catalyst wherein at least about 50% of the copper is the copper(II) oxidation state.
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Page/Page column 15
(2008/06/13)
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- Pharmaceutical aminophosphonic acid derivatives
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Aminophosphonates alpha substituted by phenol groups, of formula (I) have lipoprotein(a) lowering activity.
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- 8-arylalkyl- and 8-arylheteroalkyl-5,11-dihydro-6H-dipyrido?3,2-B:2',3'-e!?1!diazepines and their use in the treatment of HIV-1 infection
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Disclosed are novel 8-arylalkyl-5,11-dihydro-6H-dipyrido?3,2-b:2',3'-e!?1,4!diazepines. These are useful in the treatment of HIV-1 infection.
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- 8-Arylalkyl- and 8-arylheteroalkyl-5, 11-dihydro-6H-dipyrido-[3,2-b:2', 3'-e][1,4]diazepines and their use in the prevention or treatment of HIV infection
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The invention relates to novel 8-arylalkyl-5,11-dihydro-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepines of general formula 1 which are useful in the prevention or treatment of HIV infection.
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- PREPARATION OF NEW 2-CHLORO-5-FLUORO-6-(4-PHENYL-METHYLPIPERAZINYL)-4-TRIFLUOROMETHYL-3-NICOTINIC ACID
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The nicotinic acid (15), which could be a key intermediate for novel potential antibacterial 1,8-naphthyridine-3-carboxylic acid analogues, was prepared initiating with construction of the pyridine nucleus by ethyl 2-fluoroacetate and ethyl 2-trifluoroacetate.
- Remuzon, Philippe,Bouzard, Daniel,Jacquet, Jean-Pierre
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p. 431 - 434
(2007/10/02)
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- SYNTHESIS OF SOME 1-ALKYL-1,4-DIHYDRO-4-OXO-1,7-NAPHTHYRIDINE-3-CARBOXYLIC ACIDS
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Reaction of substituted 2-aminopyridines IIIa, IIIb, IIIe, and IIIf with ethyl ethoxymethylene malonate provided corresponding pyridylaminomethylenemalonates Va-Vd, respectively.Thermal cyclization of Va, Vc, and Vd yielded substituted ethyl 4-hydroxy-1,7-naphthyridine-3-carboxylates VIa, VIc, and VId.Compounds VIc and VId treated with morpholine have 8-morpholino derivatives VIe and VIf.These compounds were ethylated to mixtures of N-ethylated (VIIa, VIIb) and O-ethylated products (VIIIa, VIIIb).Compound VIIIb was also prepared from ethyl 4-chloro-6-fluoro-8-morpholino-1,7-naphthyridine-3-carboxylate VIIIc and sodium ethanolate.Esters VIIa and VIIb were hydrolyzed under acidic conditions to the respective acids VIIc and VIId.
- Radl, Stanislav,Hradil, Pavel
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p. 2420 - 2429
(2007/10/02)
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- REDUCTION OF HETERO-AROMATIC NITRO COMPOUNDS WITH BAKER'S YEAST
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Reduction of nitro group on hetero-aromatics with baker's yeast has been examined.
- Takeshita, Mitsuhiro,Yoshida, Sachiko
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p. 2201 - 2204
(2007/10/02)
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