- Self-powered continuous nitration method and device
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The invention belongs to the technical field of organic synthesis application, and particularly relates to a self-powered continuous nitration method and device. According to the method, a raw material (or a raw material solution) and mixed acid (or nitric acid) are added into a self-powered continuous reactor at the same time, reaction feed liquid continuously and circularly flows, is mixed and reacts in a tube pass through self-propelling force generated by stirring of an impeller, the mass and heat transfer process is completed, and the target requirement is met. According to the invention, the mass transfer and heat transfer efficiency can be improved, the heat exchange and heat transfer capabilities are improved, the reaction time is shortened, the risk degree of art is reduced, the thermal runaway risk is avoided, the reaction safety is improved, and the realization of chemical industry intrinsic safety large scale production is facilitated.
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Paragraph 0053-0056
(2021/07/17)
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- Novel nitrating process of 3-nitro-4-chlorobenzotrifluoride
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The invention discloses a novel nitrating process of 3-nitro-4-chlorobenzotrifluoride. A used catalyst is a biodegradable ionic liquid with a quaternary ammonium cation structure; raw materials are p-chlorobenzotrifluoride and ammonium nitrate; nitration reaction is carried out under the action of the catalyst, so that the 3-nitro-4-chlorobenzotrifluoride is obtained. Compared with the prior art,the novel nitrating process of the 3-nitro-4-chlortrifluorotoluene, provided by the invention, has the advantages that (1) ammonium nitrate is adopted to replace nitric acid, so that the 3-nitro-4-chlorobenzotrifluoride is wide in raw material source, convenient to use, and less in equipment corrosion; (2) the ion liquid can be biodegraded, so that the 3-nitro-4-chlorobenzotrifluoride is environmentally friendly; (3) the ion liquid replaces concentrated sulfuric acid, so that the novel nitrating process of the 3-nitro-4-chlortrifluorotoluene is an environment-friendly chemical process, and hasa favorable industrial application prospect.
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Paragraph 0019; 0021; 0026; 0027; 0029
(2018/09/21)
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- Novel nitration process of 3,5-binitro-4-chlorobenzotrifluoride
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The invention discloses a novel nitration process of 3,5-binitro-4-chlorobenzotrifluoride. The novel nitration process comprises the following steps: mixing nitrate, fuming sulfuric acid and a waste acid according to a ratio so as to obtain a mixed acid, performing a dinitration reaction with 4-chlorine-3-nitro trifluorotoluene in a reaction kettle, after the completion of a reaction, performing phase separation so as to obtain a semi-waste acid and a target compound, applying the semi-waste acid to mononitratio reaction on p-chlorobenzotrifluoride, performing phase separation so as to obtaina waste acid and a mononitratio compound, treating the waste acid in a waste acid kettle, performing a dinitration reaction on the treated waste acid, and further recycling the waste acid. Compared with the prior art, the novel nitration process is capable of reducing and eliminating pollution from sources, is an environmental-friendly chemical process and has good industrial application prospects.
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Paragraph 0018-0019; 0022-0023
(2018/09/08)
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- Inexpensive NaX (X = I, Br, Cl) as a halogen donor in the practical Ag/Cu-mediated decarboxylative halogenation of aryl carboxylic acids under aerobic conditions
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Versatile and practical Ag/Cu-mediated decarboxylative halogenation between readily available aryl carboxylic acids and abundant NaX (X = I, Br, Cl) has been achieved under aerobic conditions in moderate to good yields. The halodecarboxylation is shown to be an effective strategy for S-containing heteroaromatic carboxylic acid and benzoic acids with nitro, chloro and methoxyl substituents at the ortho position. A gram-scale reaction and a three-step procedure to synthesize iniparib have been performed to evaluate the practicality of this protocol. A preliminary mechanistic investigation indicates that Cu plays a vital role and a radical pathway is involved in the transformation.
- Fu, Zhengjiang,Jiang, Ligao,Zuo, Qianming,Li, Zhaojie,Liu, Yanzhu,Wei, Zhenhong,Cai, Hu
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supporting information
p. 5416 - 5421
(2018/08/12)
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- Synthetic method of aryl halide taking aryl carboxylic acid as raw material
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A synthetic method of an aryl halide taking aryl carboxylic acid as a raw material is characterized in that a corresponding aryl halide is formed by carrying out substitution reaction on an aryl carboxylic acid compound and haloid salt MX in an organic solvent under the condition that oxygen, a silver catalyst, a copper additive and a bidentate nitrogen ligand exist, wherein M in MX represents alkali metal or alkaline earth metal, and X represents F, Cl, Br or I. Compared with a conventional aryl halide synthetic method, the synthetic method disclosed by the invention has the obvious advantages that reaction raw materials (comprising aryl carboxylic acid and MX) are cheap and easy to obtain, the using amount of a metal catalyst is small, pollution to the environment when the oxygen is used as an oxidant is the smallest, good tolerance to various functional groups on an aromatic ring is obtained, the yield is high, and the like. The synthetic method disclosed by the invention can be widely applied to synthesis in the fields of medicine, materials, natural products and the like in industry and academia.
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Paragraph 0091
(2018/01/03)
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- Research on controllable degradation of sulfonylurea herbicides
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In order to seek ecologically safer and environmentally benign sulfonylurea herbicides (SU), insight into the structure/bioassay/soil degradation tri-factor relationship was first established. With the introduction of various groups (alkyl, nitro, halogen, cyano etc.) at the 5th position of its benzene ring, structural derivatives of chlorsulfuron were designed, synthesized, and evaluated for their herbicidal activity. The structures of the title compounds were confirmed by infrared spectroscopy, ultraviolet spectroscopy, 1H and 13C NMR, mass spectrometry, elemental analysis and X-ray diffraction. Bioassay results confirmed that most derivatives retained their superior herbicidal activities in comparison with chlorsulfuron. After investigating the soil degradation behavior of each molecule under set conditions, it was found that structures with electron-withdrawing substituents at the 5th position of the benzene ring retained their long degradation half-lives, yet the introduction of electron-donating substituents accelerated the degradation rate. These results will provide a valuable clue to further explore the potential controllable degradation of SU and other herbicides, and to discover novel herbicides that are favorable for environmentally and ecologically sustainable development.
- Hua, Xue-Wen,Chen, Ming-Gui,Zhou, Shaa,Zhang, Dong-Kai,Liu, Ming,Zhou, Sha,Liu, Jing-Bo,Lei, Kang,Song, Hai-Bin,Li, Yong-Hong,Gu, Yu-Cheng,Li, Zheng-Ming
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p. 23038 - 23047
(2016/03/12)
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- Decarboxylative Halogenation and Cyanation of Electron-Deficient Aryl Carboxylic Acids via Cu Mediator as Well as Electron-Rich Ones through Pd Catalyst under Aerobic Conditions
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Simple strategies for decarboxylative functionalizations of electron-deficient benzoic acids via using Cu(I) as promoter and electron-rich ones by employing Pd(II) as catalyst under aerobic conditions have been established, which lead to smooth synthesis of aryl halides (-I, Br, and Cl) through the decarboxylative functionalization of benzoic acids with readily available halogen sources CuX (X = I, Br, Cl), and easy preparation of benzonitriles from decarboxylative cyanation of aryl carboxylic acids with nontoxic and low-cost K4Fe(CN)6 under an oxygen atmosphere for the first time.
- Fu, Zhengjiang,Li, Zhaojie,Song, Yuanyuan,Yang, Ruchun,Liu, Yanzhu,Cai, Hu
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p. 2794 - 2803
(2016/04/26)
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- Conversion of aromatic amino into trifluoromethyl groups through a Sandmeyer-type transformation
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A novel strategy for aromatic trifluoromethylation by converting amino into trifluoromethyl groups via a Sandmeyer-type reaction is reported. The transformation involves diazotization of the aromatic amines with tert-butyl nitrite and hydrochloric acid to form aryldiazonium chlorides, followed by trifluoromethylation with trifluoromethylsilver at low temperature. Various readily available aromatic amines are smoothly converted under mild conditions. Georg Thieme Verlag Stuttgart. New York.
- Wang, Xi,Xu, Yan,Zhou, Yujing,Zhang, Yan,Wang, Jianbo
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supporting information
p. 2143 - 2148
(2014/08/18)
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- Silver-mediated trifluoromethylation of aryldiazonium salts: Conversion of amino group into trifluoromethyl group
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A novel strategy for aromatic trifluoromethylation by converting aromatic amino group into CF3 group is reported herein. This method, which can be considered as trifluoromethylation variation of the classic Sandmeyer reaction, uses readily available aromatic amines as starting materials and is performed under mild conditions.
- Wang, Xi,Xu, Yan,Mo, Fanyang,Ji, Guojing,Qiu, Di,Feng, Jiajie,Ye, Yuxuan,Zhang, Songnan,Zhang, Yan,Wang, Jianbo
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supporting information
p. 10330 - 10333
(2013/08/23)
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- Synthesis, biological evaluation, and molecular docking studies of 2,6-dinitro-4-(trifluoromethyl)phenoxysalicylaldoxime derivatives as novel antitubulin agents
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A series of 2,6-dinitro-4-(trifluoromethyl)phenoxysalicylaldoxime derivatives (1h-20h) have been designed and synthesized, and their biological activities were also evaluated as potential antiproliferation and tubulin polymerization inhibitors. Among all the compounds, 2h showed the most potent activity in vitro, which inhibited the growth of MCF-7, Hep-G2 and A549 cell lines with IC50 values of 0.70 ± 0.05, 0.68 ± 0.02 and 0.86 ± 0.05 μM, respectively. Compound 2h also exhibited significant tubulin polymerization inhibitory activity (IC50 = 3.06 ± 0.05 μM). The result of flow cytometry (FCM) demonstrated that compound 2h induced cell apoptosis. Docking simulation was performed to insert compound 2h into the crystal structure of tubulin at colchicine binding site to determine the probable binding model. Based on the preliminary results, compound 2h with potent inhibitory activity in tumor growth may be a potential anticancer agent.
- Zhao, Ting-Ting,Lu, Xiang,Yang, Xian-Hui,Wang, Li-Ming,Li, Xi,Wang, Zhong-Chang,Gong, Hai-Bin,Zhu, Hai-Liang
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experimental part
p. 3233 - 3241
(2012/07/14)
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- Syntheses and bioactivity of o- or p-trifluoromethylphenyl phosphates
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o- and p-Trifluoromethylphenyl phosphates designed as mechanism-based phosphotyrosine phosphatase inactivators have been prepared. Some of them show herbicidal activities.
- Zhou, Xinming,He, Yantao,Wang, Miao,Ding, Yixiang
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scheme or table
p. 651 - 659
(2009/11/30)
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- Monoazo dyes, process for their preparation, and the use thereof
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The invention relates to monoazo dyes of the formula STR1 wherein K is the radical of a coupling component of the benzene, naphthalene or heterocyclic series, and R is hydrogen, halogen, carboxy, a C1 -C6 alkyl, C1 -C6 alkoxy, C2 -C6 alkanoylamino, C1 -C6 alkylsulfonylamino, C1 -C6 alkylsulfonyl, phenyl(C1 -C4)alkylsulfonyl or naphthyl(C1 -C4)alkylsulfonyl or benzoyl radical, which radicals may be further substituted, or is a STR2 group, wherein each of R1 and R2 independently of the other is hydrogen or a C1 -C6 alkyl, C5 -C7 cycloalkyl, phenyl or naphthyl radical, which radicals may be further substituted, and wherein X is hydrogen, halogen or a C1 -C6 alkyl, C1 -C6 alkoxy, C2 -C6 alkanoylamino or C1 -C6 alkylsulfonylamino radical, which radicals may be further substituted. These dyes give dyeings of good light- and wetfastness properties on polyamide material.
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- Process for the halogenation, nitration and fluorination of aromatic derivatives
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A process for the halogenation (bromination or chlorination)/nitration/fluorination of aromatic derivatives substituted by at least one group containing a halogenoalkyl unit. The aromatic derivative is reacted with a halogen and a nitrating agent in liquid hydrofluoric acid. The products obtained are useful as intermediates for the synthesis of compounds having a plant-protecting or pharmaceutical activity.
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