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    • 33. 发明授权
    • Controlled feed process for making 3, 5-diaminobenzotrifluoride
    • 制备3,5-二氨基三氟甲苯的控制进料方法
    • US5629449A
    • 1997-05-13
    • US930942
    • 1992-08-17
    • David E. Albright, Jr.
    • David E. Albright, Jr.
    • B01J23/44C07B61/00C07C209/36C07C211/52C07C209/32
    • C07C211/52C07C209/365
    • Disclosed is a method of making 3,5-diaminobenzotrifluoride from 4-chloro-3,5-dinitrobenzotrifluoride. A solution of 4-chloro-3,5-dinitrobenzotrifluoride in an alcohol is prepared. Separately, a slurry is prepared of a palladium catalyst on a suitable substrate, at least one equivalent of magnesium oxide per equivalent of 4-chloro-3,5-dinitrobenzotrifluoride, sufficient hydrogen-donating reducing agent to reduce the 4-chloro-3,5-dinitrobenzotrifluoride to 3,5-diaminobenzotrifluoride, and an amount of alcohol sufficient to make the slurry stirrable. The solution is added to the slurry with stirring at a rate that does not exceed the reaction rate of the 4-chloro-3,5-dinitrobenzotrifluoride so that no unreacted 4-chloro-3,5-dinitrobenzotrifluoride accumulates in the slurry. The reaction mixture is heated at about 75.degree. to about 100.degree. C.
    • 公开了从4-氯-3,5-二硝基三氟甲苯制备3,5-二氨基三氟甲苯的方法。 制备4-氯-3,5-二硝基三氟甲苯在醇中的溶液。 另外,在合适的底物上制备钯催化剂的浆液,每当量的4-氯-3,5-二硝基三氟甲苯至少一当量的氧化镁,足够的供氢还原剂以还原4-氯-3, 5-二硝基三氟甲苯至3,5-二氨基三氟甲苯,以及足以使浆料搅拌的量的醇。 将溶液以不超过4-氯-3,5-二硝基三氟甲苯的反应速率的速度搅拌加入到浆料中,使得浆料中不会积聚未反应的4-氯-3,5-二硝基三氟甲苯。 将反应混合物在约75℃至约100℃加热
    • 34. 发明授权
    • Process for preparing 3,5-difluoroaniline
    • 制备3,5-二氟苯胺的方法
    • US5294742A
    • 1994-03-15
    • US032986
    • 1993-02-18
    • Thomas SchachTheodor Papenfuhs
    • Thomas SchachTheodor Papenfuhs
    • B01J23/44C07B61/00C07C17/00C07C17/093C07C25/13C07C205/12C07C209/36C07C211/52
    • C07C209/365C07C17/093C07C201/12
    • Process for preparing 3,5-difluoroaniline, wherein(1) 2,4,5-trichloronitrobenzene is reacted with an alkali metal fluoride in the presence or absence of a polar aprotic solvent at temperatures of about 100.degree. C. to about 250.degree. C., and, after filtering off precipitated salts and fractional distillation of the crude solution,(2) the resulting 5-chloro-2,4-difluoronitrobenzene is chlorinated with denitration to give 1,3-dichloro-4,6-difluorobenzene in the absence of a Lewis acid or of another chlorination catalyst, using anhydrous chlorine gas at temperatures of about 80.degree. to about 250.degree. C., and(3) this compound is nitrated to give 2,6-dichloro-3,5-difluoronitrobenzene in oleum with mixed acid (sulfuric acid/nitric acid) at temperatures of about 15.degree. to about 80.degree. C., and(4) this compound is reduced with hydrogen in the presence of palladium as catalyst and in the presence of an inorganic or organic base at temperatures of about 40.degree. to about 250.degree. C.
    • 制备3,5-二氟苯胺的方法,其中(1)在约100℃至约250℃的温度下,在极性非质子溶剂存在或不存在下,将2,4,5-三氯硝基苯与碱金属氟化物反应 在过滤沉淀的盐并分解粗溶液后,(2)将所得的5-氯-2,4-二氟硝基苯用脱硝进行氯化,得到1,3-二氯-4,6-二氟苯 在约80℃至约250℃的温度下使用无水氯气,并且(3)将该化合物硝化,得到2,6-二氯-3,5-二氟硝基苯 在约15℃至约80℃的温度下使用混合酸(硫酸/硝酸)的发烟硫酸,和(4)该化合物在钯作为催化剂存在下并在无机或有机物存在下用氢还原 碱在约40度至约2℃的温度下进行 50摄氏度
    • 37. 发明授权
    • Catalytic reduction of dinitrobenzenes using a noble metal catalyst and
iron or iron salts
    • 使用贵金属催化剂和铁或铁盐催化还原二硝基苯
    • US5105012A
    • 1992-04-14
    • US595901
    • 1990-10-11
    • George Theodoridis
    • George Theodoridis
    • C07C209/36
    • C07C209/365
    • There is provided an improved process for the reduction of optionally substituted dinitrobenzenes to the corresponding nitroanilines with high yields which comprises contacting the dinitrobenzene with hydrogen in an acidic medium in the presence of a catalytic amount of a combination of a noble metal hydrogenation catalyst, and iron or an iron salt. Isomer specific reductions may be achieved with those compounds containing suitable directing substituents.The 2-halo-5-nitroanilines which may be produced in this process may be converted via a multi-step synthesis to useful 1-aryl-4-substituted 1,4-dihydro-5H-tetrazol-5-one herbicides.
    • 提供了一种用于以高收率将任选取代的二硝基苯还原成相应的硝基苯胺的改进方法,其包括在催化量的贵金属氢化催化剂和铁的组合存在下,在酸性介质中使二硝基苯与氢接触 或铁盐。 可以通过含有合适导向取代基的那些化合物来实现异构体特异性降低。 可以在该方法中生产的2-卤代-5-硝基苯胺可以通过多步合成转化为有用的1-芳基-4-取代的1,4-二氢-5H-四唑-5-酮除草剂。