• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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    • 专利摘要:

    公开号:SU795460A3
    申请号:SU792771699
    申请日:1979-06-06
    公开日:1981-01-07
    发明作者:Шредер Хорст；Голиаш Карл；Бек Уве
    申请人:Байер Аг (Фирма)；
    IPC主号:
    专利说明:

    (54) METHOD FOR OBTAINING 2-OXIMINOPHENYLACETONITRILE
    权利要求:
    Claims (2)
    [1]
    The invention relates to an improved process for the preparation of a derivative of oximinophenyl, in particular to a method for the preparation of 2-ximinophenylacetonitrile, which can be used as an intermediate in the synthesis of pesticides materials. A known method for ps-radiation of 2-hydroxy-minophenylacetonitrile of the formula is that, at 10-8 ° C, the benzyl cyanide is reacted with alkyl nitrite in the presence of VII alkaline alcohol in anhydrous lower aliphatic alcohol, followed by acidification of the reaction mixture l. The disadvantage of this method is that the yield of the target product is 69%. The aim of the invention is to increase the yield of the target product. This goal is achieved by the method of obtaining 2-oximino-phenylacetonitrile by reacting benzyl cyrone at 10-80 s in the presence of a base in a medium of aliphatic alcohol, followed by acidification of the reaction mixture and the separation of the target product, the distinguishing feature of which is an aqueous solution of sodium hydroxide and the process is conducted in an aqueous alcohol environment. The oxidation reaction proceeds exothermically, it is carried out at 1080 ° C, preferably 20-40 ° C. The molar ratio of benzyl cyanide and alkyl nitrite is 1: 1-1: 1.2, preferably 1: 1-1: 1.15, and molar the ratio of benzyl cyanide and caustic soda can be 1: 1-1: 1.5, preferably 1: 1-1: 1.3. Acidification of the reaction mixture is carried out at, preferably 40-60 ° C. Alkyl nitrite is preferably used with alkyl nitrite with 1-5 carbon atoms. The proposed method allows to increase the yield of the target product to 91%. The invention is illustrated by the examples below. Example 1, To a solution of 980 g of methanol, 480 g of 50% aqueous sodium hydroxide and 468 g of benzyl cyanide at 35-45 ° C for 2-4 hours, 290 g of methyl nitrite are introduced. Stir for half an hour at 35-45 ° C and dilute with 7 g of ice water. The reaction mixture is adjusted to pH 2-3 with the addition of hydrochloric acid. The resulting oximinofenil acetonitrile is filtered and washed with water. Yield 545 g (93.3% of theory) | eximinophenylacetonitrile with a pure {100%. Example
    [2]
    2. To a solution of 70 g of isopropanol 130 g of 40% aqueous sodium hydroxide solution and 114 g of benzylcyavid at 25–35 ° C for 8–10 h give 105 g of isopropyl nitrite. The reaction mixture is adjusted to pH 2-3 by addition of hydrochloric acid. Excess isopropyl nitrite and isopropanol are distilled off in vacuo. The resulting oximinophenylacetonitrile is filtered at 20 ° C and washed with water. The yield is 122 g (86% of theory) of oxyminophenylacetonitrile with a purity of 100%. Example 3. To a solution of 475 g of methanol, 215 g of water, 126 g of sodium hydroxide, and 279 g of benzyl cyanide at 3040-s for. 4-5 hours in 167 g of methyl nitrite. Stir for about 35 ° C. Add saline to a pH of 2–3 and raise the temperature to 55-60 ° C. The reaction mixture is fed to 4 liters of ice water for half an hour. The resulting oximinophenylacetonitrile is filtered and washed with water. Yield 317 g (91% of theory) of oxyminophenyl acetonitrile with a purity of 100%. Example 4. 200 kg / h of methanol, 80 kg / h of 50% aqueous sodium hydroxide, 60 kg / h of water, and 94 kg / h of benzyl cyanide at 30–40 ° C are reacted with each other. The reaction solution is fed in a circle using a pump, and an injector is used which sucks 54 kg / h of methyl nitrite. The reaction is carried out without pressure. After diluting with water and acidifying with sulfuric acid, the resulting hydroxyminophenyl acetonitrile is filtered and washed with water. The yield is 105 kg / h (90% of theory) of oxyminophenylacetonitrile with 100% purity. The invention method for producing 2-oxyminophenylacetonitrile by reacting benzyl cyanide with alkyl nitrite in the presence of base at 10-U-B-C in an environment of lower aliphatic alcohol, followed by acidifying the reaction mixture and isolating the desired product, which is An aqueous solution of caustic soda is used as a base and the process is conducted in an aqueous alcohol medium. Sources of information taken into account during the examination 1 .1. T. Thurston-Preparation of alkylation and acylation of. Alts of phenylnitroacetonitrile.2, 1938, c. 192-193 (prototype).
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    同族专利:
    公开号 | 公开日
    EP0006152A1|1980-01-09|
    DE2825565A1|1979-12-20|
    EP0006152B1|1980-11-12|
    HU176923B|1981-06-28|
    DD144259A5|1980-10-08|
    JPS54163548A|1979-12-26|
    PL216181A1|1980-03-10|
    US4233233A|1980-11-11|
    IL57507D0|1979-10-31|
    CS207794B2|1981-08-31|
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    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2749358A|1955-02-18|1956-06-05|Du Pont|Preparation of oximes|
    US3090812A|1959-09-24|1963-05-21|Nepera Chemical Co Inc|Method of producing isonitrosopropiophenone|
    FR2054700A5|1969-07-23|1971-05-07|Rhone Poulenc Sa|US4824476A|1985-06-24|1989-04-25|Ciba-Geigy Corporation|Herbicidally active derivatives of N-phenyl-3,4,5,6-tetrahydrophthalimide|
    DE3607300A1|1986-03-06|1987-09-10|Basf Ag|N-ARYLTETRAHYDROPHTHALIMIDE DERIVATIVES AND THEIR PRE-PRODUCTS|
    US5629442A|1993-07-02|1997-05-13|Shionogi & Co., Ltd.|Process for producing α-hydroxyiminophenylacetonitriles|
    DE69410414T2|1993-07-02|1998-12-10|Shionogi & Co|METHOD FOR PRODUCING CARBONIC ACID DERIVATIVES|
    TWI511965B|2010-06-28|2015-12-11|Bayer Ip Gmbh|Process for the preparation of 5-substituted 1-alkyltetrazolyl oxime derivatives|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE19782825565|DE2825565A1|1978-06-10|1978-06-10|PROCESS FOR THE PREPARATION OF 2-OXIMINOPHENYL ACETONITRILE|
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