One pot synthesis of <Emphasis Type="Italic">N</Emphasis>-ethylaniline from nitrobenzene and ethanol

A novel method for the one pot synthesis of N-alkyl arylamines from nitro aromatic compounds and alcohols is proposed through the combination of the aqueous-phase reforming of alcohol for hydrogen production, the reduction of nitro aromatic compounds for the synthesis of aromatic amine and the N-alkylation of aromatic amine for the production of N-alkyl arylamine over an identical catalyst under the same conditions of temperature and pressure in a single reactor. In this process, hydrogen generated from the aqueous-phase reforming of alcohols was used in-situ for the hydrogenation of nitro aromatic compounds for aromatic amine synthesis, followed by N-alkylation of aromatic amine with alcohols to form the corresponding N-alkyl arylamines at a low partial pressure of hydrogen. For the system composed of nitrobenzene and ethanol, under the conditions of 413 K and P _N2 = 1 MPa, the conversion degrees of nitrobenzene and aniline were 100%, the selectivity to N-ethylaniline and N, N-diethylaniline were 85.9% and 0%–4%, respectivity, after reaction for 8 h at the volumetric ratio of nitrobenzene:ethanol:water = 10:60:0. The selectivity for N, N-diethylaniline production is much lower than that through the traditional method. In this process, hydrogen and aromatic amines generated from the aqueous-phase reforming of alcohols and hydrogenation of nitro aromatic compounds, respectively, could be promptly removed from the surface of the catalyst due to the occurrence of in-situ hydrogenation and N-alkylation reactions. Thus, this may be a potential approach to increase the selectivity to N-alkyl arylamine. Supported by the Program for New Century Excellent Talents in University (Grant No. NCET-04-0557), and the Specialized Research Fund for the Doctoral Program of High Education (Grant No. SRFDP-20060337001)     

One pot and solvent-free synthesis of 2,9,16,23-tetrachlorometal(II) phthalocyanines

A novel one pot and solvent-free synthesis of 2,9,16,23-tetrachloro metal(II)phthalocyanines in microwave using monosodium salt of 4-chlorophthalate as starting material is described. This method in comparison to conventional route offers high yields (75–92%), eliminates the use of toxic organic solvents, reduces multistep synthesis to one-step, reaction temperature from 190 to 120°C, and reaction time from 5–6 hours to 5 minutes.     

One pot synthesis and gelation studies of amphiphilic triblock polyurethanes

This article shows a generalized synthetic strategy to make amphiphilic ABA type triblock polyurethane (PU) in a SINGLE reaction pot. This is achieved by condensation polymerization between a hydrophobic diol and a di‐isocyanate in the presence of a polyethylene glycol monomethyl ether (M_w = 2000 or 5000 g mol^?1) as mono‐functional impurity. Using different ratios of the three reactants with a fixed parameter such that the total concentration of –OH = isocyanate, a series of PUs are produced with both the ends capped with PEG. These polymers show facile gelation ability in solvents like dimethyl formamide, dimethyl sulfoxide, and dimethyl acetamide by H‐bonding interaction among the urethane groups. A comprehensive structure–property relationship study reveals importance of the right balance between the weight fractions of the soft and hard segments in self‐assembly and efficient gelation. © 2014 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014 , 52, 2502–2508     

One pot synthesis of bis-silicon-bridged stilbene derivatives

Bis-silicon-bridged stilbene derivatives were synthesized in a modified procedure that combined the preparation of bis[2- (silyl)phenyl]acetylene and its intramolecular reductive cyclization in one pot.The results indicated that the one pot approach produced target products in a comparable yield to that of the two-step method reported previously.     

A new one pot and solvent-free synthesis of nickel porphyrin complex

Abstract

A new one pot and solvent-free synthesis of nickel porphyrin complex is described. This is prepared by condensing pyrrole, benzaldehyde, nickel (II) chloride, and 1,8-diazabicyclo [5.4.0] undec-7-ene as a base. This new method allows higher yields, reduced reaction times, ease of handling, and follows principles of green chemistry. The same complex is also prepared by an alternative route, i.e. first, the porphyrin is prepared and then the insertion of metal ion.     

One pot synthesis of dibenzodiazepinones via CuI catalysis in ethylene glycol

A one pot protocol for the synthesis of dibenzodiazepinones was developed.The substituted ethyl 2-halobenzoates are cross-coupled with o-phenylenediamine utilizing a ligand-free,CuI catalyzed system,which spontaneously undergo an intramolecular N-acylation in ethylene glycol to give the corresponding products in high yields.This synthetic protocol provides a concise and efficient access to a wide variety of dibenzodiazepinone,including biologically active molecules.     

One pot synthesis of some new N-allyl and N-benzyl quinazolinones and their anti-inflammatory activity

The simple and more reliable one-pot synthesis of some novel compounds of allyl/Benzyl quinazolinone (4aa-4bd) with good yields from readily available derivatives of anthranilic acid and benzoyl chloride was also reported. Interestingly, as compared to Diclofenac sodium, compounds 4ac, 4ad, 4ba, 4bc and 4bd displayed remarkable anti-inflammatory activity (Scheme 1 & Table 2).     

A convenient route toward one‐pot multicomponent synthesis of spirochromenes and pyranopyrazoles accelerated via quinolinic acid

In the present work, the catalytic activity of quinolinic acid (QUIN) was studied for the synthesis of spirochromene and pyranopyrazole derivatives from readily available materials. The salient features of these one‐pot multicomponent protocols are the clean reaction profile, easy isolation of products, no chromatographic separation techniques, high efficiency, short reaction time, and high yield of products plus using QUIN as a new, inexpensive, commercially available, and efficient organocatalyst.     

Synthesis of Poly(N-ethylaniline) Nanoparticles Synthesis and Characterization of Organically Soluble Conducting Poly(N-ethylaniline) Nanoparticles using Acrylic Acid as a Soft Template

In this paper, we report the synthesis of poly(N-ethylaniline) (PNETA) by using tartaric acid (TA) as an organic acid dopant by aqueous polymerization method of N-ethylaniline using ammonium per sulphate (APS) as an oxidant and acrylic acid (AA) as a soft template. This is a new polymerization method for the direct synthesis of the emeraldine salt form of poly(N-ethylaniline) in bulk quantity, which is soluble in organic solvents such as m-cresol and N-methyl pyrrolidinone. The prepared polymers were characterized by UV, FTIR, XRD, TGA, SEM and conductivity measurement studies. The results are discussed with reference to HCl doped poly(N-ethylaniline). It is observed that PNETA/TA/AA polymer is comparatively more soluble in m-cresol than that doped with HCl in its salt form. The formation of emeraldine salt phase and dopping process was confirmed by FTIR and UV-Vis spectroscropy. We demonstrate the effect of organic dopant on the morphology and conductivity of the PNETA. It was found that, PNETA doped with TA synthesized using acrylic acid (AA) as a soft template display higher doping level, crystallinity and solubility in common organic solvent. On the contrary, HCl doped polymer was lowered at doping level and amorphous in nature which reflects the role of organic dopant and soft template. X-ray diffraction studies indicate that the PNETA/TA/AA doped samples exhibit higher crystallinity, which indicates enhanced polymer sub-chain alignment as compared to HCl doped polymer. This is also manifested by the FTIR studies. SEM result also revealed the continuous morphology and sub-micrometer size, evenly distributed particles of the PNETA/TA/AA doped polymer.     

One‐pot synthesis of block copolymers by ring‐opening polymerization and ultraviolet light‐induced ATRP at ambient temperature

We successfully synthesized poly(l ‐lactide)‐b‐poly (methyl methacrylate) diblock copolymers at ambient temperature by combining ultraviolet light‐induced copper‐catalyzed ATRP and organo‐catalyzed ring‐opening polymerization (ROP) in one‐pot. The polymerization processes were carried out by three routes: one‐pot simultaneous ATRP and ROP, one‐pot sequential ATRP followed by ROP, and one‐pot sequential ROP followed by ATRP. The structure of the block copolymers is confirmed by nuclear magnetic resonance and gel permeation chromatography, which suggests that the polymerization method is facile and attractive for preparing block copolymers. © 2018 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2018 , 56, 699–704     

One‐pot synthesis of trifluoromethylated benzimidazolines catalyzed by phosphotungstic acid with a low catalyst loading

The inexpensive Keggin‐type polyoxometalate, i.e. H₃PW₁₂O₄₀ was found to be an effect catalyst for the condensation‐cyclization reaction of 1,2‐phenylenediamines and trifluoromethyl ketones to synthesize trifluoromethylated heterocycles, including benzimidazolines, benzoxazolines and benzothiazolines. Only 1 mol% of H₃PW₁₂O₄₀ was required in this work, and the synergistic effect of proton and polyanion was vital for the reaction. Significantly, the POM catalyst could be easily recovered by using a biphasic solvent system (H₂O/toluene, V/V = 1:5), and reused at least for four times without significant loss in activity.     

A mild and efficient one pot synthesis of 1,3,4-oxadiazoles from carboxylic acids and acyl hydrazides

A convenient one pot method for the synthesis of 2,5-disubstituted 1,3,4-oxadiazoles from acids and acyl hydrazides is reported. Acid activation with CDI, followed by coupling with the desired acylhydrazide and dehydration in the same pot with Ph₃P and CBr₄ affords the corresponding 1,3,4-oxadiazoles in good yield. The scope of the acid and acylhydrazide components is presented.     

碲氢化钠存在下3－氧代硫代羧酸酯的一步合成法

３－氧代硫代羧酸酯可由α－溴代酮与碲氢化钠作用形成的烯醇盐与二硫代碳酸二乙酯进行乙氧硫代羰基化反应制得。３－氧代硫代羧酸酯的烯醇含量可由核磁共振谱测得     

Protecting‐group‐free synthesis of glycopolymers bearing thioglycosides via one‐pot monomer synthesis from free saccharides

Polyacrylamides having pendant thioglycosides were successfully synthesized from thioglycosidic monomers that were readily prepared by one‐pot method without any protection of the hydroxy groups on the starting free saccharides. The glycomonomers were synthesized by the direct synthesis of thioglycosides using 2‐chloro‐1,3‐dimethylimidazolinium chloride and 4‐aminobenzentiol, and the following acrylamidation. They were co‐polymerized with acrylamide into glycopolymers by reversible addition‐fragmentation chain transfer polymerization using a trithiocarbonate derivative as a chain transfer agent. The gold nanoparticles and gold‐coated quartz crystal microbalance sensor immobilized with the thiol‐terminated glycopolymers exhibited high affinity for the corresponding lectins due to multivalent interaction between saccharides and protein in aqueous solution. © 2014 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014 , 52, 3513–3520     

A convenient one‐pot method for the synthesis of symmetrical dialkyl trithiocarbonates using NH4OAc under mild neutral conditions

A facial, new, one‐pot method for the preparation of symmetrical organic trithiocarbonates from various alkyl halides and carbon disulfide is described. This is a convenient, clean, and mild procedure, which involves the use of the neutral, nontoxic, commercially available, and inexpensive reagent NH₄OAc in the preparation of the trithiocarbonate ion from carbon disulfide.     

原位液相催化加氢法合成N-乙基苯胺和N，N-二乙基苯胺

以硝基苯为原料,Pt/γ-Al2O3为催化剂,乙醇水溶液为溶剂和氢供体,采用原位液相加氢一步法合成了N-乙基苯胺和N,N-二乙基苯胺.采用低温N2吸附-脱附、电感耦合等离子体发射光谱、X射线衍射、程序升温化学吸附和透射电子显微镜等对Pt/γ-Al2O3催化剂进行了表征,并考察了所制备催化剂的原位液相加氢性能.结果表明,在温度为503K、压力为5.0MPa、空速为3.2h-1、溶剂水含量为30%以及硝基苯浓度为8%的反应条件下,在Pt/γ-Al2O3催化剂上原位液相加氢合成N-乙基苯胺及N,N-二乙基苯胺有较好的结果,硝基苯转化率达到100%,N-乙基苯胺和N,N-二乙基苯胺的总收率达到99.5%.讨论了硝基苯原位液相加氢合成N-乙基苯胺和N,N-二乙基苯胺的反应机理.     

"一锅法"合成5-氟-2-羟基-苯乙酮

对合成5-氟-2-羟基-苯乙酮的方法进行改进,将原来的两步反应合并为一步,去掉了中间产物酯的繁琐分离和纯化,大大缩短了反应时间,操作简便,收率88．9％,适用于工业化生产。     

One‐pot synthesis of composite microspheres with core‐shell structure

One‐pot synthesis of thermoresponsive magnetic composite microspheres with a poly(N‐isopropylacrylamide) (PNIPAM) shell and a Fe₃O₄ core is demonstrated. Temperature sensitivity of PNIPAM was adopted to design the novel synthesis pathway. The as‐prepared composite microspheres have an obvious core‐shell structure with a mean size of approximately 250 nm. The Fe₃O₄ core is approximately 5 nm and the thickness of the PNIPAM shell is approximately 10 nm. The content of Fe₃O₄ in the composite microspheres can be controlled by this method. The composite microspheres experience a swelling and shrinking process in water by adjusting the temperature below and above the lower critical solution temperature (LCST) around 32 °C. These microspheres also show fine response to an external magnetic field. This work presents a platform to synthesize organic/inorganic composite microspheres in a facile and efficient approach. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2013, 51, 2702–2708     

Sn‐mediated one‐pot four‐component allylation of aldimines

A convenient and facile method for the synthesis of homoallylic amines was disclosed. The one‐pot reaction of aldehydes, aromatic amines and allylic bromide with tin powder at room temperature could afford the homoallylic amines in good to excellent yield without any promoter or additive. The method is highly efficient and environmentally benign with low cost and concise manipulation. Copyright © 2014 John Wiley & Sons, Ltd.