• 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 4-KITRODIFENIPASNA formula by reacting 4-nitrochlorobenzene of formula ci with an aniline formJFII 40 W in an organic solvent in the presence of potassium carbonate and copper oxide (I), characterized in that, to increase the yield of the target product with a single reduction In the process, the latter is carried out in the presence of a cesium salt with weak organic or high amic acid. sc
    公开号:SU1158038A3
    申请号:SU833673464
    申请日:1983-12-12
    公开日:1985-05-23
    发明作者:Вилли Мюллер Эрнст
    申请人:Байер Аг (Инопредприятие)；
    IPC主号:
    专利说明:

    1 The invention relates to methods for producing nitrodiphenipamines, in an hour of the bone, to methods for producing 4-nitrodiphenylamine. The purpose of the invention is to increase the yield of the target product while reducing the duration of the process. Example 1. In a 2-liter three-flask flask equipped with a stirrer and a distillation apparatus with a water separator, at a stirring speed of 400 revolutions per minute, I fed 1 mol of 4-chloronitrobenzene, 1.9 mol of aniline, 1.25 mol of dry potassium carbonate, 1/42 mol of copper (II) oxide, 1/950 mol of dry cesium carbonate and 1/10 mol of xylene. The reaction mixture with stirring, is heated to 195 ° C. The contents of the flask are maintained at this temperature until 10 to 10.5 ml of water are released and then the sample is subjected to liquid chromatography to determine the content of 4-chloronitrobenzene. If this content is less than 1.5% of the initial amount, the reaction is stopped by cooling. Otherwise, the reaction is continued until 382 is reached. The total reaction time is 5-6 hours. With 50 ml of water is added and the volatile components are stripped off with steam. The aqueous phase of the contents of the flask is separated, and the organic phase solidifies upon cooling. 216 g of a gray-green substance are obtained, containing according to the data of liquid chromatography 86% by weight of 4-nitrodiphenylamine, which, in terms of 4.-chloronitrobenzene, corresponds to a yield equal to 87%. Example 2. Example 1 is repeated, with the difference that 1/930 moles of cesium cyanide are used instead of cesium carbonate. 4-nitrodiphenylamine is obtained. The yield is 88.7% (in terms of 4-chloronitrobenzene). Example 3. Example Ic is repeated, with the difference that 1.95 mol of aniline, 1.3 mol of potassium carbonate, 1/45 mol of copper (II) oxide, 1/850 mol of acetate, 1/20 mol of water and 1/12 are used. mole of xylene and distilled II ml of water. The yield of 4-nitrodiphenylamine, in terms of 4-nitrolorbenzene, is 89.2%.
    权利要求:
    Claims (1)
    [1]
    METHOD FOR PRODUCING 4-NITRO DIPHENYLAMINE of the formula by reaction of 4-nitrochlorobenzene of the formula ci with aniline of the formula
    MH 2 5
    0 | s in an organic solvent medium - in the presence of potassium carbonate and copper (II) oxide, characterized in that, in order to increase the yield of the target product while reducing the duration of the process, the latter is carried out in the presence of a cesium salt with a weak, organic or inorganic acid .
    1 1158038 2
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    同族专利:
    公开号 | 公开日
    BR8306844A|1984-07-24|
    JPS59112947A|1984-06-29|
    JPS6323184B2|1988-05-16|
    KR910002370B1|1991-04-20|
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    KR840007560A|1984-12-08|
    IN160179B|1987-06-27|
    CS236898B2|1985-05-15|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    RU2502724C1|2012-10-22|2013-12-27|Российская Федерация, От Имени Которой Выступает Министерство Промышленности И Торговли Российской Федерации|Method of producing nitrodiphenylamines|NL211629A|1955-12-07|
    DE1056619B|1956-11-29|1959-05-06|Bayer Ag|Process for the preparation of 4-nitro-diarylamines|
    DE1090225B|1957-11-05|1960-10-06|Us Rubber Co|Process for the preparation of p-nitrodiphenylamines|
    US3155727A|1960-07-25|1964-11-03|Goodyear Tire & Rubber|Reaction of aromatic amines with para halo nitrobenzenes using copper cyanide condensation catalyst|
    US3313854A|1961-11-20|1967-04-11|Universal Oil Prod Co|Preparation of para-nitrodiphenylamines utilizing a copper oxide catalyst|
    US3277175A|1963-11-26|1966-10-04|Eastman Kodak Co|Preparation of p-nitrodiphenylamines|
    US4187248A|1977-11-23|1980-02-05|Monsanto Company|Making a nitrodiarylamine by reacting an alkali metal salt of a formamide with a nitrohaloarene|
    US4209463A|1977-12-27|1980-06-24|Monsanto Company|Promoting the formation of nitrodiarylamines from nitrohaloarenes, activated aryl amines and sodium carbonates|
    US4187249A|1977-12-27|1980-02-05|Monsanto Company|Promoting the reaction of sodium salts of formyl derivatives of aromatic amines to form nitrodiarylamines|
    US4228103A|1978-03-13|1980-10-14|Monsanto Company|Effecting condensation of nitrohaloarene and formyl derivative of a primary aromatic amine with alkali metal hydroxide|DE19942394C1|1999-09-06|2001-02-01|Bayer Ag|Increasing the yield of nitrodiphenylamines in base/palladium-catalysed nitrohalobenzene/aromatic amine reactions by using a base which has been milled and optionally also dried|
    DE10005601A1|2000-02-09|2001-08-16|Bayer Ag|Process for the preparation of aminodiphenylamines|
    DE10300126A1|2003-01-07|2004-07-15|Bayer Aktiengesellschaft|Process for the preparation of aminodiphenylamines|
    DE10300125A1|2003-01-07|2004-07-15|Bayer Ag|Process for the preparation of nitrodiphenylamines|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE3246151A|DE3246151C2|1982-12-14|1982-12-14|
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