• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    A process for the dechlorination of aromatic nitro or amino compounds comprising reacting anilines or nitrobenzenes, which are polysubstituted by chlorine, with hydrogen, under the action of heat, in the presence of an excess of chloride ions, in the liquid phase and at low pressure. The process makes it possible selectively to obtain anilines which are chlorine-substituted in the meta-position.
    公开号:SU1082316A3
    申请号:SU802882799
    申请日:1980-02-14
    公开日:1984-03-23
    发明作者:Кордье Жорж
    申请人:Рон-Пуленк Агрошими (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to an improved method for producing
    3,5-dichloroaniline, which is used in various fields of the chemical industry (pharmacology, 5 production of polymeric materials, etc.).
    Closest to the proposed is a method for producing 3,5-dichloroaniline by hydrogenation of the corresponding 10- or tetrachloranilines in an acidic aqueous medium (10 N solution of hydrochloric acid with the addition of sulfuric acid) in the presence of palladium on activated carbon at 250 ° C and 15 at 200 atm (ratio of concentrations 1 --- j <1). The yield of the target product is 89% [1].
    The disadvantages of this method are the insufficiently high yield 20 of the target product and the complexity of the process associated with the use of high pressure (200 atm) and elevated temperature (250 ° C).
    The invention aims to 25 cheyaie increase the yield and simplification of the process.
    This goal is achieved by the fact that according to the method for producing 3,5 dichloroaniline by hydrogenation of trichloro- 30 or tetrachloroanilines containing chlorine atoms in positions 3 and 5, in the presence of palladium on carbon and lithium chloride in 4 n, an aqueous solution of hydrochloric acid at a ratio of centrations equal to 2, pressure bar and temperature of 170 ° C. The yield of the target product is 95.4%.
    The positive effect of the proposed method consists in increasing the yield of the target product (by 6.4%) and simplifying the process, which is expressed in a significant reduction in operating pressure (from 200 bar to 21 bar) and lowering the process temperature (with
    250 to 170 ° C) those. reduction of energy costs for the process.
    Example 1. In an autoclave with a capacity of 225 cm 3 having an inner coating of tantalum, load 0.83 g
    2.3.4.5 - tetrachloroaniline, 0.07 g of the catalyst, which is palladium on activated carbon (specific surface area of the carrier 1100 m 2 / g, weight content of palladium 10%), 95 cm of an aqueous solution of hydrochloric acid with a concentration of 4 mol / l (4 n, ) and 16.1 g of lithium chloride.
    The autoclave is closed, purged first with argon, then with hydrogen. Then heated to 170 ° C, when this temperature is reached, hydrogen is introduced to a total pressure of 21 bar, of which 8 bar is the partial pressure of hydrogen. Under these conditions, the process is carried out for 4 hours 10 minutes.
    After which the reaction mixture is cooled, alkalinized with an aqueous solution of soda (NaOH), the palladium catalyst is separated by filtration,
    3.5-dichloroaniline was extracted from the aqueous phase with methylene chloride, the solution thus obtained in methylene chloride was dried over sodium sulfate, and the solvent was evaporated in vacuo. The conversion of tetrachloroaniline is 100%. The yield of 3.5 dichloroaniline is 95.4%.
    Examples 2-4. Under the conditions of Example 1, starting from 2,3,5,6-tetrachloro, 2,3,5-trichloro or 3,4,5-trichloroaniline, the desired product is obtained in a yield of 95.4 + 0.1%.
    The technical and economic efficiency of the proposed method for producing 3 ,, 5-dichloroaniline is to increase the yield of the target product and simplify the process (a significant decrease in the operating parameters of the process - pressure and temperature).
    权利要求:
    Claims (1)
    [1]
    METHOD FOR PRODUCING 3,5-Dichloroaniline by hydrogenation of trichloro- or tetrachlororanilines containing chlorine atoms no 1 in positions 3 and 5, in the presence of palladium on activated carbon and hydrochloric acid under heating and elevated pressure, characterized in that, in order to increase the yield of the target product and simplification of the process, the process is carried out at a total pressure of 21 bar and a temperature of 170 ° C in a 4 N aqueous solution of hydrochloric acid in the presence of lithium chloride at a concentration ratio [crj „
    ----- g is equal to 2.
    [H + ]
    108,231 6
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    同族专利:
    公开号 | 公开日
    YU42323B|1988-08-31|
    DK153392B|1988-07-11|
    YU37880A|1983-01-21|
    DK62880A|1980-08-16|
    ES488572A1|1980-10-01|
    DK153392C|1988-11-28|
    IT8047892D0|1980-02-13|
    IL59190A|1983-06-15|
    IL59190D0|1980-05-30|
    IE49393B1|1985-10-02|
    AT372370B|1983-09-26|
    NL8000620A|1980-08-19|
    ATA85480A|1983-02-15|
    SE8001166L|1980-08-16|
    BR8000910A|1980-10-29|
    FR2449077B2|1983-04-29|
    GB2042542B|1983-05-05|
    CH642049A5|1984-03-30|
    DE3003960C2|1990-07-05|
    DE3003960A1|1980-08-28|
    CA1139313A|1983-01-11|
    GB2042542A|1980-09-24|
    SE447897B|1986-12-22|
    IT1127360B|1986-05-21|
    DD149060A5|1981-06-24|
    FR2449077A2|1980-09-12|
    US4324914A|1982-04-13|
    IE800277L|1980-08-15|
    HU185214B|1984-12-28|
    LU82167A1|1981-09-10|
    JPS5928544B2|1984-07-13|
    JPS55149229A|1980-11-20|
    BE881754A|1980-08-18|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US3148217A|1961-11-16|1964-09-08|Gen Aniline & Film Corp|Catalytic hydrogenation of halonitrobenzene compounds|
    DE2032565A1|1970-07-01|1972-01-05|Farbwerke Hoechst AG, vormals Meister Lucius & Bruning, 6000 Frankfurt|Process for the preparation of 3 difluorochloromethylanines|
    DE2036313C3|1970-07-22|1982-03-25|Bayer Ag, 5090 Leverkusen|Process for the preparation of halogen-substituted aromatic amines|
    CS188122B2|1971-02-08|1979-02-28|Kurt Habig|Method of production the sulfide catalysts with the platinum on coal|
    DE2503187C3|1975-01-27|1979-05-31|Bayer Ag, 5090 Leverkusen|Process for the preparation of chlorine-meta-substituted anilines|
    FR2403990B1|1977-09-22|1983-01-21|Rhone Poulenc Agrochimie|
    DE2758111B2|1977-12-24|1980-10-16|Basf Ag, 6700 Ludwigshafen|DE3127026A1|1981-07-09|1983-01-20|Bayer Ag, 5090 Leverkusen|METHOD FOR PRODUCING M-CHLORINE-SUBSTITUTED ANILINE|
    FR2521132B1|1982-02-05|1984-03-16|Rhone Poulenc Agrochimie|
    US4888425A|1982-04-30|1989-12-19|Union Carbide Chemicals And Plastics Company Inc.|Preparation of polyalkylene polyamines|
    JPH0433781B2|1982-09-27|1992-06-04|Mitsui Toatsu Chemicals|
    JPS62132400U|1986-02-14|1987-08-20|
    USRE34745E|1986-10-30|1994-09-27|The Dow Chemical Company|High purity process for the preparation of 4,6-diamino-1,3-benzenediol|
    US5001279A|1989-11-17|1991-03-19|The Dow Chemical Company|Aqueous synthesis of 2-halo-4,6-dinitroresorcinol and 4,6-diaminoresorcinol|
    US5294742A|1992-03-21|1994-03-15|Hoechst Atkiengesellschaft|Process for preparing 3,5-difluoroaniline|
    US8956378B2|2008-02-29|2015-02-17|Cook Biotech Incorporated|Coated embolization device|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR7904483A|FR2449077B2|1979-02-15|1979-02-15|
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