• 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:
    METHOD FOR OBTAINING 3,5-DICHLORANILINE by hydrogenating tri- or tetrachloroanilines, necessarily containing chlorine in positions 3 and 5, in the presence of palladium on activated carbon, hydrochloric acid and catalytic amounts of metal salt 1b-5a of the Periodic System with heating and elevated pressure , characterized in that, in order to simplify the process, a metal chloride selected from the group is used as the metal salt: bismuth (III), tin (II), thallium
    公开号:SU1149871A3
    申请号:SU802882800
    申请日:1980-02-14
    公开日:1985-04-07
    发明作者:Кордье Жорж
    申请人:Рон-Пуленк Агрошими (Фирма)；
    IPC主号:
    专利说明:


    WITH
    00

    one
    The invention relates to preservative. A novel method for the preparation of 3,5-dichloraniline, which is used as a starting compound in various fields of organic chemistry, including for the synthesis of medical preparations and herbicides.
    The closest to the invention is a method for producing 3,5-dichloroaniline by hydrogenating polychloroanilines, necessarily containing chlorine atoms in positions 3 and 5, in the presence of palladium on activated carbon and catalytic amounts of metal sulfides 1c-5a of subgroups of the Gyrogodic system (in particular, silver (1), lead (II), iron (II), cobalt (II), nickel (II), manganese (II), cadmium (II) or antimony (II), taken in an amount, Providing a concentration of metal not less than 0.1 g-at / l, in a 2M-aqueous solution of hydrochloric acid at 150-260 0 and d 200 atm occurrence of the expected product Yield -. Close to quantitative lj..
    The disadvantage of this method is the complexity of the wires, the process unit associated with the use of high pressures (200 atm).
    The aim of the invention is to simplify the process of producing 3,5-dichloroaniline.
    This goal is achieved by the fact that according to the method of producing 3,5-dushoraniline by hydrogenating tri- or tetrachloroanilines, necessarily containing chlorine atoms in positions 3 and 5, in the presence of palladium on activated carbon and catalytic amounts of metal chloride 1b-5a subgroups. Periodic system at heating and elevated pressure, metal chloride selected from bismuth (III), tin (II), thallium (1), mercury (II), and silver sulfate (1) or lead sulfate ( P), taken in an amount, provided a metal concentration of 0.001-0.05 g x pat / l, and the process was carried out at a total pressure of 13 bar in 4/4 - aqueous hydrochloric acid solution.

    Examples 1-6i .. A 250 cm autoclave having an inner coating of tantalum is loaded with 0.416 g of 2,3,4,5-tetrachloroaniline, 5 0.14 g of catalyst, which is palladium on activated carbon (the specific surface of the carbon black 1100, weight content of palladium 10%), 120 cm of a 4H-aqueous O hydrochloric acid solution, a metal salt, taken in an amount such that the concentration g-at / l of this metal (in the cationic state) would be equal to in table 15, the autoclave is closed, purged first with argon and then with hydrogen. After that, it is heated to, leaving the autogenous pressure to increase, then, when this temperature reaches 0, hydrogen is introduced to a total (relative) pressure of 13 bar, of which 6 bar is the partial pressure of hydrogen,
    Under these conditions, the reaction is carried out for the period indicated in the table. Cool the liquid reaction mass, alkalify with an aqueous solution of soda or NaOH, separate the catalyst by filtration,
    0 3,5-dichloroaniline is extracted from the aqueous phase with methylene chloride, the solution thus obtained in methylene chloride is dried over sodium sulfate, the solvent
    5 is evaporated in vacuo, In various. in the examples, the degree of conversion of tetrachloroaniline is 100%,
    The resulting yield of 3,5-dichloroaniline for each example is presented in the table.
    Similar results were obtained for hydrogenation under the conditions of Examples 1-6 2,3,5- and 3,4,5-trichloroanilines and 2,3,5,6-tetrachloroaniline.
    5 (the yield of the target products 92-98%, the duration of the process 2,337, 5 hours).
    The technical and economic efficiency of the proposed method is to simplify the process by significantly reducing the operating pressure from 200 bar to 13 bar (13 bar), which allows the process to be carried out in low or medium pressure autoclaves.
    0,005
    Tlcl
    0.05
    Pbsq,
    0,005
    SnClj
    0,005 BiCl AgjSOl
    0,005
    0,001 HgCl2
    96,8
    30 min 95.7
    30 min 92.7 98.4
    30 mcn 98.1 55 min 97.8 30 min
    权利要求:
    Claims (1)
    [1]
    METHOD FOR PRODUCING 3,5-Dichloroaniline by hydrogenation of tri- or tetrachlororanilines, which necessarily contain chlorine atoms in positions 3 and 5, in the presence of palladium on activated carbon, hydrochloric acid and catalytic amounts of metal salt of subgroups 1b-5a of the Periodic System under heating and high pressure, which differs in order to simplify the process, metal chloride is used as a metal salt of a metal selected from the group: bismuth (W), tin (P), thallium (1) mercury (Π), as well as silver sulfate (1) or lead sulfate (Π) taken in quantity, both ensures, metal concentration of 0.001-0.05 g * khat / l, and the process is carried out at a total pressure of 13 bar in the water-containing medium 4N hydrochloric acid solution.
    1 1149871
    类似技术:
    公开号 | 公开日 | 专利标题
    US4409395A|1983-10-11|Process for the production of glycollic acid esters
    US2499172A|1950-02-28|Process for converting lower-boiling ketones into higher-boiling ketones
    US3873597A|1975-03-25|2-Bromo-2-bromomethylglutaronitrile
    RU2127253C1|1999-03-10|Process for preparing 2-alkyl-6-methyl-n-|aniline and 2-alkyl-6-methyl-n-|-n-chloroacetanilide
    SU1149871A3|1985-04-07|Method of obtaining 3,5-dichloraniline
    JPH0525101A|1993-02-02|Preparation of aniline
    US4729977A|1988-03-08|Supported catalyst, process for its preparation and its use for the preparation of hydroxydiphenyl
    US3654365A|1972-04-04|Process for the preparation of para-aminophenol
    SU1082316A3|1984-03-23|Process for preparing 3,5-dichloroaniline
    US3048634A|1962-08-07|Production of ketoximes
    SU1176830A3|1985-08-30|Method of producing 3,5-dichloroaniline
    US5053564A|1991-10-01|Selective hydrogenolysis of perhalogenated ethane derivatives
    SU1199199A3|1985-12-15|Method of producing 3,5-dichloraniline
    US4054588A|1977-10-18|Process for the preparation in a single stage of saturated omega-aminoacids from olefinically unsaturated omega-aldehydoacids
    US4239928A|1980-12-16|Process for preparing alkyl-substituted aromatic compounds
    US3427355A|1969-02-11|Process for preparing aniline and alkyl aniline
    NL8220298A|1983-07-01|IMPROVED PREPARATION METHOD OF INDOLE.
    US4045484A|1977-08-30|Process for preparing N'-methyl acethydrazide
    US4297509A|1981-10-27|Process for preparing alkali metal salts 3-amino-2, 5-dichlorobenzoic acid
    US3989743A|1976-11-02|Process for the preparation of 4,4'-diaminostilbene-2,2'-disulphonic acid
    US3132180A|1964-05-05|Catalytic reduction of aromatic mononitro compounds
    US4161615A|1979-07-17|Dehydrogenation of cyclic ketones to beta-naphthols
    SU1313342A3|1987-05-23|Method for producing beta-oxypropionic acid amide
    EP0056615B1|1984-06-13|Process for the preparation of carnitinamide
    US4611069A|1986-09-09|Process for preparing gamma-caprolactone by isomerization of epsilon-caprolactone
    同族专利:
    公开号 | 公开日
    DK153391C|1988-11-28|
    FR2449076B2|1983-05-20|
    DD149061A5|1981-06-24|
    AT1006T|1982-05-15|
    JPS55149232A|1980-11-20|
    EP0015220A1|1980-09-03|
    US4340759A|1982-07-20|
    ES488570A1|1980-10-01|
    GB2043066A|1980-10-01|
    IE49885B1|1986-01-08|
    IL59191A|1983-06-15|
    BR8000911A|1980-10-29|
    HU185213B|1984-12-28|
    CA1139315A|1983-01-11|
    DK62780A|1980-08-16|
    IE800276L|1980-08-15|
    YU38080A|1983-01-21|
    EP0015220B1|1982-05-12|
    FR2449076A2|1980-09-12|
    DE3060394D1|1982-07-01|
    JPS5848542B2|1983-10-28|
    DK153391B|1988-07-11|
    YU42206B|1988-06-30|
    IL59191D0|1980-05-30|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US3666813A|1969-08-27|1972-05-30|Engelhard Min & Chem|Process for preparing aromatic haloamines from aromatic nitroamines|
    BE792080A|1971-11-30|1973-05-29|Rhone Progil|DEHALOGENATION OF POLYHALOGENOUS AROMATIC COMPOUNDS|
    DE2503187C3|1975-01-27|1979-05-31|Bayer Ag, 5090 Leverkusen|Process for the preparation of chlorine-meta-substituted anilines|FR2487824B1|1980-08-01|1984-08-24|Rhone Poulenc Agrochimie|
    IL63297A|1980-08-01|1984-05-31|Rhone Poulenc Agrochimie|Selective preparation of meta-chloroanilines|
    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|
    FR2532305B1|1982-08-24|1984-12-07|Rhone Poulenc Agrochimie|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR7904482A|FR2449076B2|1979-02-15|1979-02-15|
    [返回顶部]