- Novel process for synthesizing 2 -cyano -4 -nitrochlorobenzene by continuous nitration through solvent method
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The invention provides a novel process for synthesizing 2 -cyano -4 -nitrochlorobenzene by continuous nitration through a solvent method, which comprises the following steps: preparing a phthalonitrile solution; dissolving o-chlorobenzonitrile with an organic solvent; and preparing a phthalonitrile solution for standby. The method comprises the following steps: preparing a mixed acid nitration agent. Step III: nitration reaction: the phthalonitrile solution in the step and the mixed acid nitration agent in the step two are respectively pumped into the nitration reactor, and nitration reaction is carried out to generate the nitration liquid. The method comprises the following steps: mixing the nitration liquid in the three steps with water, adding the secondary solvent to mix evenly, and carrying out phase separation treatment. To the invention, 2 - cyano -4 - nitro - chlorobenzene solution in the step is subjected to evaporation treatment, the evaporation residue is 2 - cyano -4 - nitrochlorobenzene product, the waste acid amount generated in the reaction process is greatly reduced, the safety risk level is reduced by adopting the continuous nitration reaction, and the product yield is improved.
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Paragraph 0049-0056
(2021/10/11)
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- Method and device for preparing 2-chloro-5-nitrobenzonitrile in pipeline
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The invention discloses a method and a device for preparing 2-chloro-5-nitrobenzonitrile in a pipeline. The device comprises a storage tank, a nitrogen oxide steel cylinder, an ozone generator, a flowpump, a gas flowmeter, a reaction pipeline filled with a catalyst, a mixer, a cooling system, a heating system, a backpressure valve and a receiving tank. The method comprises the following steps: dissolving a raw material 2-chlorobenzonitrile in an organic solvent and adding the mixture into the storage tank; opening the cooling system and the heating system; opening the ozone generator and adjusting the backpressure value; mixing the raw material 2-chlorobenzonitrile and nitrogen dioxide through the mixer and feeding the mixture into the reaction pipeline for a nitrification reaction; and carrying out post-treatment to obtain 2-chloro-5-nitrobenzonitrile. The method is simple to operate, mild in reaction condition, quick to transfer mass and heat, simple in post-treatment, high in safety and good in economical benefit, the catalyst can be repeatedly used, and the method is a green and environment-friendly process suitable for industrial production.
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Paragraph 0010; 0045-0048; 0049-0051; 0052-0054; 0055-0060
(2019/03/08)
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- Micro-reaction preparation process 2 -amino -5 - nitrotoluene carbonitrile (by machine translation)
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The invention discloses a micro-reaction preparation process, 2 - amino -5 -nitrobenzaldehyde. The process comprises the following steps: a. heating o-chlorobenzonitrile to liquid through a water bath; b. adding liquid o-chloronitrile - organic inert solvent solution and mixed acid in step a to an organic inert solvent; c, conveying o-chlorobenzonitrile to the micro reaction module through a high-pressure infusion pump; dwell 60 - 150S discharging the reaction product unitarily by a temperature control system. b. A 55 - 75 °C temperature control system The reaction product is washed to neutrality by a sodium hydroxide solution and distilled water; e, the solvent, obtained 2 - chlorine -5 - nitrosobutyronitrile; f. in step e is 2 - added -5 - to a high-pressure reaction kettle; and then the 2 - high -5 -pressure reaction kettle is used for pressure relief to collect excess liquid ammonia and separating chlorobenzene and reaction products 2.5h; and the solvent is distilled and recovered by a compression pump; and chlorobenzene and reaction products are separated. J. The reaction product in step i is washed and then dried. (by machine translation)
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Paragraph 0026-0031; 0038-0043; 0050-0055
(2019/08/01)
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- Synthetic process of 2-cyano-4-nitroaniline
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The invention relates to a synthetic process of 2-cyano-4-nitroaniline, comprising the following steps: putting chlorobenzonitrile into a sulfuric acid medium, dropwise adding mixed acid for nitration, adding water for elutriation of a nitrated object, then filtering the nitrated object, dissolving a nitrated material in chlorobenzene, performing an ammonolysis reaction by nitre-chlorine mixed fluid and liquid ammonia, then distilling to recycle a solvent, performing suction filtration, and washing to be neutral, thus obtaining a wet product. The process is simple in step and easy to control, the obtained product is high in yield, high in purity and stable in quality, and has an environmental index capable of meeting the market need, the cost is low, sewage is little, energy consumption is reduced, and the synthetic process is a production process low in energy consumption and low in pollution.
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Paragraph 0019; 0020; 0021
(2016/10/24)
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- New nitration technology used in production of 2-cyano-4-nitro chlorobenzene
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The invention belongs to the field of chemical industry, and relates to a new nitration technology used in production of 2-cyano-4-nitro chlorobenzene. The new nitration technology takes o-chlorobenzonitrile as a raw material and uses mixed acid prepared from medium-concentration sulfuric acid and medium-concentration nitric acid as a solvent, and comprises the steps of dissolving the o-chlorobenzonitrile by using the solvent, and carrying out a nitration reaction at the medium temperature. The new nitration technology completely overcomes the defects that in the traditional technology, the electric energy consumption is high since high-concentration sulfuric acid and high-concentration nitric acid are used for carrying out the nitration reaction at low temperature, and the quality of the 2-cyano-4-nitro chlorobenzene is reduced if the temperature is slightly high.
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Paragraph 4; 5
(2017/07/21)
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- Palladium-catalyzed highly selective ortho-halogenation (I, Br, Cl) of arylnitriles via sp2 C-H bond activation using cyano as directing group
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A palladium-catalyzed ortho-halogenation (I, Br, Cl) of arylnitrile is described. The optimal reaction conditions were identified after examining various factors such as catalyst, additive, solvent, and reaction temperature. Using cyano as the directing group, the halogenation reaction gave good to excellent yields. The method is compatible to the arylnitriles with either electron-withdrawing or electron-donating groups. The reaction is available to the substrate in at least gram scale. The present method was successfully applied to the synthesis of the precursors of paucifloral F and isopaucifloral F.
- Du, Bingnan,Jiang, Xiaoqing,Sun, Peipei
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p. 2786 - 2791
(2013/04/24)
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- AMIDE COMPOUNDS AND MEDICINAL USE THEREOF
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The present invention relates to a compound of the formula wherein R1 is substituted aryl, heteroaryl and the like, R2 and R3 are hydrogen, alkyl, halogen, hydroxyl group and the like, Q is N, CH and the like, W is hydrogen, alkyl, hydroxycarbonylalkyl and the like, X is halogen, cyano, nitro, amino and the like, X' is hydrogen, halogen, cyano, nitro, and Y is alkyl, hydroxyl group, alkoxy, mercapto and the like and a salt thereof, and a medicine containing the said compound. The compound of the present invention shows a superior inhibitory effect on activated lymphocytes proliferation and is useful as an agent for the prophylaxis or treatment of various autoimmune diseases.
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- Aniline derivatives
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N-formyl anilino aromatic compounds containing two electronegative groups in the benzene ring, their manufacture from formanilides and aromatic halogen compounds and their use as intermediates for the manufacture of the corresponding diphenylamine compounds. The compounds are useful as pesticides.
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- Tricyclic Systems Obtained from Some 3-Aminobenzothiophen Derivatives
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4-Hydroxybenzothienopyridin-2(1H)-one (3) was obtained by cyclisation of a benzothiophen derivative containing either 2-CO2Et, 3-NH.CO.CH2.CO2Et or 2-CO.CH2.CO2Et, 3-NH2 substituents. 3-Amino-2-formyl-, 3-amino-2-acetyl-, and 3-amino-2-acetyl-5-nitro-benzothiophens were converted into the corresponding 3-thiocyanato-compounds, which gave tricyclic systems when treated with hydroxylamine.Heating these with polyphosphoric acid gave benzothienoisothiazole, and its 3-methyl and 3-methyl-7-nitro-derivatives respectively.Nitration, formylation, and oxidation reactions of 3-methylbenzothienoisothiazole have been investigated.
- Clarke, Kenneth,Fox, William Richard,Scrowston, Richard M.
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p. 833 - 847
(2007/10/02)
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- Process for the preparation of nitriles
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A process for the preparation of a nitrile of the formula wherein R represents an optionally substituted alkyl, cycloalkyl or aryl radical or an optionally substituted 5- or 6-membered heterocyclic radical which may additionally be fused with a benzene ring and n' represents 1 to 6 which comprises contacting a carboxylic acid of the formula wherein R and n' have the meanings given above with cyanogen chloride and/or cyanogen bromide at a temperature in the range of 100° to 300° C.
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