• 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:
    1. A process for the preparation of substantially pure pyrazole compounds of the general formula see diagramm : EP0012216,P9,F1 where R is hydrogen, halogen, alkyl of up to 5 carbon atoms, alkoxy of up to 3 carbon atoms, perhaloalkyl of up to 3 carbon atoms or alkoxyalkyl of up to 5 carbon atoms, R**1 is hydrogen, halogen, alkyl of up to 5 carbon atoms, alkoxy of up to 3 carbon atoms, perhaloalkyl of up to 3 carbon atoms or alkoxyalkyl of up to 5 carbon atoms, R**2 is hydrogen, halogen, alkyl of up to 5 carbon atoms, alkoxy of up to 3 carbon atoms, perhaloalkyl of up to 3 carbon atoms or alkoxyalkyl of up to 5 carbon atoms, or R**2 together with R is an ortholinked alkylene chain of up to 6 carbon atoms which is unsubstituted or substituted by alkyl of up to 4 carbon atoms, X is chlorine or bromine, and R**3 and R**4 are identical or different and each is hydrogen, alkyl, alkoxy, alkylthio, carbalkoxy or perfluoroalkyl, in each case of up to 4 carbon atoms, or halogen, phenyl, cyano or carboxyl, from the corresponding crude products, characterized in that the crude products are treated with 30 to 90% by weight aqueous solutions of strong acids, thereafter the aqueous solution is separated off and diluted with water, and the pure product which hereupon precipitates is separated from the aqueous fluid.
    公开号:SU860699A1
    申请号:SU792841459
    申请日:1979-11-12
    公开日:1981-08-30
    发明作者:Линхарт Фридрих；Эйкен Карл；Гиргензон Берн；Рихарц Винфрид
    申请人:Басф Аг (Фирма)；
    IPC主号:
    专利说明:

    The aqueous aqueous solution is separated, diluted with water, taken in 5-11% of acid, and the precipitated product is separated from the aqueous medium.
    Example 1. 5100 parts by weight, N-chloromethyl-2, 6-dimethylchloroacetanilide and 11000 parts by weight toluene is mixed with 1900 weight.h. 4-methylpyraol and then stirred for 3 hours at a temperature of 40 ° C. Then 2130 parts by weight are added. triethylamine, stirred for 3 h at and during the night at room temperature (20s). The reaction mixture is washed twice with 10,000 parts by weight. water and once extracted with 12000 weight.h. 37% hydrochloric acid. The extract is served with stirring to 60000 weight.h. water and sucked precipitate. After drying 4750 parts by weight are obtained. 95% H- | 4-methylpyrazolyl- (1) -methyl-5-2, 6-dimethylchloroacetanilide, m.p. 98-100s
    Example 2. 1300 weight.h. N-chloromethyl-2-ethyl-6-methylchloroacetanilide and 3000 parts by weight. toluene is mixed with 540 weight.h. N-methoxypyrazole. Maintain for 4 hours at, add 500 parts by weight. triethylamine, stirred for 4 h at and overnight at room temperature. Mixed with 2000 weight.h. water and sucked off the precipitated at the same time the crystals, and after prolavany water and drying get 750 weight.h. pure N- 1 4-methoxypyrazolyl- (1) -methyl} -b-ethyl-2-methylchloroacetanilide with so pl. 9b-97s. The organic phase of the filtrate is separated and extracted once with 950 parts by weight. 37% hydrochloric acid. The resulting extract is added dropwise in 6000 weight.h. water After sucking off and drying the crystals that fall out in this way, 660 parts by weight of 98% N-Hmethoxypyrazolyl- (1) -methyl -2-ethyl-b-methylchloroacetanilide with m.p. 92-93 C.
    Example 3. a) 14 weight.h. 94% M-pyrazolyl- (1) -methyl -} - 2, b-dimethylchloroacetanilide with so pl. 72-75 ° C, the content of which is determined by a proton resonance spectroscope, is dissolved in 140 weight, h. toluene and extracted by shaking with 40 weight parts. 60% sulfuric acid. Sulphate extract is fed with vigorous stirring to 240 parts by weight. water, sucked off the precipitated crystals, washed with water and dried. Get 11 weight.h. 100% N- -pyraz olyl- (1) -methyl1-2 6-dimethylchloroacetanilide with so pl. .
    b) 14 weight parts 94% M-pyrazolyl (1) -methyl -2,6-dimethylchloroacetate anilide is dissolved in 140 weight parts. toluene and extracted twice, each time with 40 weight.h. 50% sulfuric acid. Conjugated
    the extract is hydrolyzed with water. The precipitation is sucked off, washed with water and dried, get 13 weight.h. 100% product with so pl. . Example 4. a) 100 weight.h. a black-brown product obtained by improperly proceeding to obtain N-Spirazolyl- (1) -methylJ-2, b-dimethylchloroacetanilide, mixed with 180 parts by weight. 37% hydrochloric acid for half an hour. After suctioning, the filtrate is extracted with 50 parts by weight. toluene and acid are added dropwise to 1000 weight.h. water. After suction and drying, 60 parts by weight are obtained. 93% M-pyrazolyl- (1) -methylJ-2, b-dimethylchloroacetanilide with so pl. .
    b) 100 weight parts. the product mentioned above (Example 4a) is well mixed and filtered with 150 parts by weight. toluene. The filtrate is extracted once by
    vstrahivan with 180 weight.h. 371% hydrochloric acid. The hydrochloric acid phase is added dropwise to 900 parts by weight. water, sucked off and dried. Get 54 weight.h. 97% N-pyrazolyl- (1) -methyl J-2, 6-dimethylchloroacetanilide with m.p. 68 ° C.
    c) 100 parts of the described (example
    4 a) the product is dissolved in 180 parts by weight of methylene chloride, extracted once with 180 and then with 60 parts by weight
    37% hydrochloric acid. The combined saltic acid extracts are washed with 50 parts by weight of methylene chloride once to remove. toluene. Subjected to hydrolysis (similar to a and b) and
    56.5 parts by weight are obtained. more than 99% of M-pyrazolyl- (1) -methylZ-2,2-dichloroacetanilide with so pl. .
    Example 5. To solution
    202 weight.h. bromoacetyl bromide
    150 weight.h. ligroin is added dropwise with a crude solution of 133 parts by weight. M- (2,6-dimethylphenyl) methyleneimine, a mixture of toluene and cyclohexane. Because instead of the desired crystalline
    M-bromomethyl-2, b-dimethyl bromoacetanilide, only difficult-to-release oil precipitates, 450 parts by weight are added. toluene and 75 weight.h. pyrazole, heated for 2 hours before, added dropwise 110 sec. triethylamine, heated to, washed with water, then with 5% hydrochloric acid and again with water and evaporated, to obtain 248 parts by weight viscous oil. This is butter
    dissolved in BOO weight.h. toluene and extracted with 250 ppmw, 37% hydrochloric acid. The extract is hydrolyzed with 1500 weight.h. water, get 190 weight.h. M-pyrazolyl- (1) -methylJ-2, 6-dimethylbromoacetanilide with
    m.p. .
    PRI m e D 6. From a mixture of 10890 weight.h. 2,6-dimethylaniline and 4050 Bec.ti. paraformaldeMide is removed from 50,000 parts by weight. mixtures of toluene and cyclohexane in a known manner
    权利要求:
    Claims (1)
    [1]
    Claim
    The method of isolation of pyrazole derivatives of General formula I
    R / CH 2 -K
    ί, s-och
    Οχ
    R and R ^ are methyl or ethyl;
    Ra is hydrogen, methyl or methoxy;
    X - chlorine or bromine, from the corresponding raw materials, characterized in that, in order to simplify the process, the raw materials are treated with 36-37% hydrochloric acid or 50-60% sulfuric acid, taken in 2-5-fold from Theoretically, the resulting aqueous solution is separated, diluted with water taken in 5-11.5-fold amount of acid, and the precipitated product is separated from the aqueous medium.
    Where
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    同族专利:
    公开号 | 公开日
    PL219574A2|1980-09-08|
    DK146534C|1984-04-09|
    AT164T|1981-09-15|
    IL58625D0|1980-02-29|
    UA7045A1|1995-03-31|
    JPS55129270A|1980-10-06|
    YU279479A|1983-01-21|
    BR7907345A|1980-07-15|
    PL119268B2|1981-12-31|
    ZA796137B|1980-11-26|
    IL58625A|1982-08-31|
    EP0012216A1|1980-06-25|
    JPH0316346B2|1991-03-05|
    DD146948A5|1981-03-11|
    CA1120043A|1982-03-16|
    DE2849442A1|1980-05-29|
    EP0012216B1|1981-08-26|
    AR226546A1|1982-07-30|
    CS208793B2|1981-09-15|
    DK146534B|1983-10-31|
    DE2960705D1|1981-11-19|
    DK481279A|1980-05-16|
    HU178450B|1982-05-28|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    DE2704281A1|1977-02-02|1978-08-03|Bayer Ag|Herbicidal N-heterocyclyl-methyl-halo-acetanilide derivs. - prepd. from a N-halomethyl-chloro:acetanilide and a heterocycle|FR2610589A1|1987-02-09|1988-08-12|Savard Franck|Directional wheel hub making it possible to give or adjust the caster independently of the caster angle, and appended systems making it possible to vary various parameters on a 2-wheeled vehicle|
    US5250503A|1989-07-29|1993-10-05|Basf Aktiengesellschaft|Monoclinic metazachlor and composition|
    DE3925253A1|1989-07-29|1991-01-31|Basf Ag|MONOCLINES METAZACHLOR AND METHOD FOR THE PRODUCTION THEREOF|
    DE4436293A1|1994-10-11|1996-04-18|Basf Ag|Stable mixture containing water and metazachlor|
    DE10210409A1|2002-03-09|2003-09-18|Feinchemie Schwebda Gmbh|Purely triclinic metazachlor and process for its manufacture|
    DE10343277A1|2003-09-18|2005-04-21|Piesteritz Stickstoff|N-amides, process for their preparation and their use as nitrification inhibitors|
    RS56792B1|2006-03-30|2018-04-30|Fmc Corp|Acetylene carbamide derivatives-polyurea polymers and microcapsules and formulations thereof for controlled release|
    WO2013104478A1|2012-01-13|2013-07-18|Basf Se|Process for preparing acetanilides|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE19782849442|DE2849442A1|1978-11-15|1978-11-15|METHOD FOR PRODUCING MOST PURE PYRAZOLIC COMPOUNDS|
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