• 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 OF OBTAINING 1,1-DIB-. ROMTETRAFTORETANE by isomerization of 1,2-dibromotetrafluoroethane using aluminum halide at a boiling point of the reaction mixture, characterized in that, in order to increase the yield and simplify the technology, aluminum chloride or aluminum bromide is used as an aluminum halide as a previously prepared catalytic complex with 1.1 .-dibromtetrafluoroethane and 1., 2-dibromtetrafluoroethane with a mass ratio of the components in the complex 1:
    公开号:SU1176826A3
    申请号:SU823503937
    申请日:1982-10-20
    公开日:1985-08-30
    发明作者:Годзо Франко；Трояни Никола；Пиккарди Паоло
    申请人:Монтэдисон С.П.А.(Фирма)；
    IPC主号:
    专利说明:

    The invention relates to: methods for raising 1,1-dibromotetrafluoroethane used 1 as an intermediate in the synthesis of pyrethroid drugs, 5
    The aim of the invention is to increase the yield and simplify the technology.
    The invention is illustrated by examples 1-3, Comparative examples 4 and 5 show the need for preliminary interaction of aluminum halide with 1,1-dibromotetrafluoroethane for the successful implementation of the method.
    Example 1. In a 1 L flask with a reflux condenser, the upper part of which is connected to a valve supplying H, 50x, the following components are introduced into the ' 2 4 20 order of magnitude: 10 g of anhydrous A1Bg g , 23 g
    1.1- dibromotetrafluoroethane, 95 g
    1.2-dibromotetrafluoroethane (ratio 1: 2.3: 9.5).
    '25
    There is a spontaneous reaction, as a result of which after 5 minutes the boiling point of the mixture is reached. At the end of the heat release, add 600 g of 1,2-dibromotetrafluoroethane, maintaining the mixture at a temperature of ^ 0 boiling.
    Samples are removed from the reaction mixture and their infrared spectrum is taken. An analysis of this spectrum shows that, after 20 minutes, the band at 9.9-10 μm, characteristic for 1,2-dibromotetrafluoroethane, completely disappears, while the intense band at 11 μm, characteristic for
    1, I-dibromotetrafluoroethane, still 40 present.
    Thus, 1200 g are added to the reaction vessel in two stages
    1,2-dibromotetrafluoroethane in the form of agr-45 gate. The ratio of aluminum bromide and ί is 1: 185.
    .'And after completion of the reaction after 40 minutes the mixture is cooled to 10 ° C, washed with 200 ml of an aqueous solution of 3% 50 alkaline sulfite and the organic phase is separated. After distillation of the organic phase, 1650 g are obtained.
    1,1-dibromotetrafluoroethane having a boiling point of 46 ° C and not containing 55-containing 1,2-dibromotetrafluoroethane “This is equivalent to a yield of 86%.
    PRI me R 2, Applied the devices and the method described in example 1. 10 g of anhydrous A1Bg 3 , 27 g of 1,1-dibromotetrafluoroethane, 105 g of 1,2-dibromotetrafluoroethane are placed in a flask. The ratio is 1: 2.7: 10.5.
    At the end of the heat evolution, 5000 g of 1,2-dibromotetrafluoroethane in the form of an aggregate are added in one step. The ratio of aluminum bromide and T is 1: 510.
    The mixture was refluxed for 3 hours and 15 minutes (during which time 1,2-dibromotetrafluoroethane completely disappeared), and then examined by the method described in Example 1, 4385 g of 1,1-dibromotetrafluoroethane were obtained. The yield of 85.6%.
    Example 3. The process is carried out as in examples 1 and 2, except that there is no pause between the stage of preparation of the catalytic complex and the introduction of the main mass of HT. Reagents are used in the following total quantities:
    3.5 g A1SC, 50 g (1.1350 g) II (ratio of aluminum chloride and TT 1: 385). Processing the reaction mixture is carried out as in examples 1 and 2. Yield T 87.4%.
    PRI me R 4. The process is carried out as in example 1, but without preliminary additives G (the stage of preparation of the catalytic complex is excluded). Within 3 hours, the reaction is not observed; output I is 0.
    II PRI me R 5. The process is conducted as in example 4, but using 26 g (2 wt.%) Anhydrous AlBr .
    The reaction mixture after 4 h at boiling point does not reveal the presence of 1,1-dib. romtetrafluoroethane.
    After another 10 hours of boiling, the mixture is treated as in Example 2, and by subsequent distillation of the organic phase, 520 g of 1,1-dibromotetrafluoroethane are obtained in a yield of 40%,
    As can be seen from examples 1-3, the method of producing 1,1-dibromotetrafluoroethane can increase the yield by 45 47% and simplify the process technology.
    权利要求:
    Claims (2)
    [1]
    1,2-dibromotetrafluoroethane using aluminum halide at the boiling point of the reaction mixture, characterized in that, in order to increase the yield and simplify the technology, aluminum chloride or bromide is used as an aluminum halide in the form of a pre-prepared catalytic complex with I, I-dib 'romtetrafluoroethane and 1.
    [2]
    , 2-dibromotetrafluoroethane with a mass ratio of components in the complex 1: (2.3-2.7) :( 9ζ5-10.5), respectively, and a mass ratio of aluminum halide and isomerized 1,2-dibromotetraftopetane 1: (185-510) .
    >
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    同族专利:
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    引用文献:
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    US2598411A|1948-11-23|1952-05-27|Atomic Energy Commission|Rearrangement of saturated halocarbons|
    US2971990A|1957-09-25|1961-02-14|Dow Chemical Co|2-bromo-1, 1, 1, 2-tetrafluoroethane|
    NL263002A|1960-03-30|1900-01-01|
    US3818229A|1970-12-21|1974-06-18|Univ Illinois|Radiopaque agents comprising brominated perfluorocarbons|
    JPS6127375B2|1977-03-30|1986-06-25|Daikin Kogyo Co Ltd|JPS6226239A|1985-05-28|1987-02-04|Du Pont|Catalytic halogen exchange of fluoroolefin|
    US4925993A|1989-06-14|1990-05-15|Dixie Chemical Company|Process for preparing chlorofluorocarbons via an in situ generated activated aluminum trichloride catalyst and products resulting therefrom|
    US5017732A|1990-02-16|1991-05-21|Dixie Chemical Company|Process for preparing chlorofluorocarbons via an in situ generated activated aluminum trihalide catalyst and products resulting therefrom|
    US5030372A|1990-07-31|1991-07-09|E. I. Du Pont De Nemours And Company|Catalytic equilibration to improve the relative yield of selected halocarbons|
    IT1251951B|1991-10-18|1995-05-27|Ausimont Spa|PROCEDURE FOR PURIFYING 1,1,1-TRIFLUORO-, 2,2 DICHLOROETHANE FROM THE ISOMER 1,1,2-TRIFLUORO-1,2-DICHLOROETANO.|
    JPH0546918U|1991-11-29|1993-06-22|中央帽子株式会社|Leather brim|
    US5416246A|1994-10-14|1995-05-16|E. I. Du Pont De Nemours And Company|Chlorofluorocarbon isomerization|
    US5523422A|1994-10-14|1996-06-04|E. I. Du Pont De Nemours And Company|Monomer precursor isomerization|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    IT2460281A|IT1139269B|1981-10-21|1981-10-21|PROCESS FOR THE PREPARATION OF 1,1-DIALO-1,2,2,2-TETRAFLUOROETANI|
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