• 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-DICHLOR ANILINE by hydrogenating tri- or tetra-chloroanilines containing chlorine atoms in 3 to 5 positions, in the presence of a palladium-based catalyst in ep (FR) organic solvent, at elevated temperatures and pressures, characterized in In order to simplify the process, the last wire is in an anhydrous medium in the presence of a catalytic amount of a Lewis acid, such as chloride. or aluminum bromide, zinc iodide, tetrachloride or dichloride TIN, iron trichloride, zinc chloride, copper or nickel. Priority by signs: 1.08.80 - using aluminum bromide as Lewis acid; 09/26/80 - the use of the remaining § of Lewis acids indicated in the formula prio.breteni5G.
    公开号:SU1176830A3
    申请号:SU813316601
    申请日:1981-08-01
    公开日:1985-08-30
    发明作者:Кордье Жорж；Фуйиу Пьер
    申请人:Рон-Пуленк Агрошими (Фирма)；
    IPC主号:
    专利说明:

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    The invention relates to an improved method for producing 3,5-dichloroaniline by hydrogenating glloranilines containing chlorine atoms in the meta position. The aim of the invention is to simplify the process. The invention is illustrated by the following examples. Example 1, In an autoclave of a 70 cm-capacitor, with an inner coating of tatal, 1.16 g of 2,3,4,5-tetrachlororaniline, 0.4 g are introduced; catalyst, from palladium precipitated on active carbon (carbon black surface area 1300, palladium content 10% by weight), 17 cm of anhydrous cyclohexane, 3 cm of 5% aluminum bromide solution (AlBr) in cyclohexane. The autoclave is closed, rinsed off with argon, then with hydrogen. After this, hydrogen is introduced at a pressure of 10 bar, the autoclave is sealed and heated to 160 ° C., and conditions are created so that the pressure spontaneously rises to the total (relative pressure of 21 bar. A chemical reaction under such conditions proceeds for 4 30 minutes The autoclave is then cooled. The contents of the autoclave are filtered to separate the solid catalyst from the hexane solution. The latter is washed with a water solution of sodium oxide (WaOH so as to completely neutralize the hydrochloric acid). 3,5-dichloroaniline with a yield of 99.5%. Example 2. The example is carried out as in Example 1 with the following autoclave charge: 1.16 g 2,3,4,5-tetrachlororaniline, 0.4 g of catalyst consisting of palladium precipitated in an amount of 5 wt .-% on the same active carbon as in example 1, 0.095 g of anhydrous tin dichloride or 0.082 parts per 1 h of tetrachloraniline), 20 cm of cyclohexane. 5-dichloroaniline with a yield of 96.5%, Example 3. The process is carried out with A1. Example 1 with the following loading, autoclave: 1 g, 2,3,4,5-tetrachloroaniline, 0.3 g of catalyst, TOGO; the same as used / in the previous example, 0.64 g of anhydrous tin dichloride. The latter is dissolved in the molten liquor at the reaction temperature (1). The reaction is continued for 3 hours and 20 minutes. Under these conditions, 3,5-dichloroaniline is obtained with a yield of 100%. EXAMPLE 4 The process is carried out as in Example 2 with the difference that 0.32 g of zinc iodide is used instead of tin dichloride. The reaction lasts 10 hours. Under these conditions, 3,5-dichloroaniline is obtained with a yield of 98.2%. Examples 5-13. Into an autoclave with a capacity of 70 cm with an inner coating of tantalum, 1 g of 2,3,4,5-tetrachloroaniline (TTCA, 0.3 g of a catalyst consisting of 3% palladium and 2% silver, deposited together on active carbon) is introduced. surface about 1300, variable amount of Lewis acid j serving as a catalyst. The reaction proceeds at 160 ° C. under a pressure of 21 bar. Treatment of the reaction medium after completion of the reaction is carried out as in Example 1. Table B shows the reaction time and yield 3.5. -dichloroaniline for every Lewis acid (L) and for a specific molar ratio of Lewis acid to tetrachloroaniline L / TTCA. Example 14. The process is carried out as in Example 1, but an equal amount of 2,3,5,6-tetrachlororaniline is used instead of 2,3,4, 5-tetrachloroaniline. 13 hours: Under these conditions, 3,5-dichloroaniline is obtained with a yield of 99.6%. Example 15. The process is carried out as in Example 1, but instead of 2,3,4,5-tetrachlorrraniline 354,5-trichloroaniline is used (0.985 g), while the Lewis acid is introduced in the form of a 1 cm cyclohexane solution with a concentration of 10% (w / v) using 0.05 g of the same palladium catalyst. The reaction proceeds for J20 min. Under these conditions, 3,5-dichloroaniline is obtained with a yield of 86%,
    权利要求:
    Claims (1)
    [1]
    METHOD FOR PRODUCING 3,5-Dichloroaniline by hydrogenation of tri- or tetrachlororanilines containing chlorine atoms in 3 and 5 positions, in the presence of a palladium-based catalyst in an organic solvent medium, at elevated temperature and pressure, characterized in that, in order to simplify of the process, the latter is carried out in an anhydrous medium in the presence of a catalytic amount of Lewis acid, such as chloride or aluminum bromide, zinc iodide, tin tetrachloride or dichloride, iron trichloride, zinc chloride, copper or nickel.
    Priority on. Signs:
    1.08.80 - the use of aluminum bromide as a Lewis acid;
    09/26/80 - the use of the remaining Lewis acids indicated in the claims *. G
    1 1176830 2
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    同族专利:
    公开号 | 公开日
    DK342981A|1982-02-02|
    IL63297A|1984-05-31|
    EP0045709A1|1982-02-10|
    IL63297D0|1981-10-30|
    HU187348B|1985-12-28|
    ES504473A0|1982-12-01|
    IE811738L|1982-02-01|
    DE3166482D1|1984-11-08|
    US4418213A|1983-11-29|
    CA1211470A|1986-09-16|
    DD201673A5|1983-08-03|
    ES8306092A1|1982-12-01|
    KR830006170A|1983-09-17|
    IE51457B1|1986-12-24|
    KR850000148B1|1985-02-28|
    BR8104979A|1982-04-20|
    EP0045709B1|1984-10-03|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    SU517576A1|1971-05-24|1976-06-15|Предприятие П/Я А-7797|Method for producing mixed haloaromatic hydrocarbons|
    DE2503187C3|1975-01-27|1979-05-31|Bayer Ag, 5090 Leverkusen|Process for the preparation of chlorine-meta-substituted anilines|
    FR2449075B1|1979-02-15|1983-03-11|Rhone Poulenc Agrochimie|
    FR2449076B2|1979-02-15|1983-05-20|Rhone Poulenc Agrochimie|FR2532305B1|1982-08-24|1984-12-07|Rhone Poulenc Agrochimie|
    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|
    US5051030A|1990-06-05|1991-09-24|Roy F. Weston, Inc.|Chemical detoxification process for treatment of soils contaminated with halogenated organic compounds|
    JPH0565250A|1991-01-28|1993-03-19|Ishihara Sangyo Kaisha Ltd|Production of 3,5-difluoroaniline|
    US5089653A|1991-04-04|1992-02-18|Dow Elanco|Process for the selective reduction of the 4-halogen in 2,4-dihaloanilines|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR8017324A|FR2487823B1|1980-08-01|1980-08-01|
    FR8020979A|FR2491059B2|1980-09-26|1980-09-26|
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