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    • 3. 发明授权
    • Synthesis of ethambutol
    • 乙胺丁醇的合成
    • US3944618A
    • 1976-03-16
    • US493802
    • 1974-08-01
    • Balwant Singh
    • Balwant Singh
    • C07C89/00C07C89/04C07C91/04
    • C07C231/10C07C233/13C07C249/02C07C257/02C07B2200/07Y02P20/582
    • D-2-Amino-1-butanol, for the synthesis of ethambutol hydrochloride, d,d'-2,2'-(ethylenediimino)di-1-butanol dihydrochloride, is produced in high purity and good yields by the reaction of butene-1, a nitrile, preferably an excess of acetonitrile, and chlorine to form N-[1-(chloromethyl)propyl]acetimidoyl chloride which is hydrolyzed to dl-2-amino-1-butanol, which can be isolated as the hydrochloride, or free base, or a mixture, resolved with L(+)-tartaric acid and the d-2-amino-1-butanol reacted with ethylene dichloride and then hydrochloric acid to form ethambutol hydrochloride. A minimum of by-products which are conveniently split out permits the economical synthesis of a pharmaceutical grade product.
    • 用于合成乙胺丁醇盐酸盐d,d'-2,2' - (乙二胺基)二-1-丁醇二盐酸盐的D-2-氨基-1-丁醇通过丁烯反应以高纯度和良好的收率生产 -1,腈,优选过量的乙腈和氯,以形成水解成dl-2-氨基-1-丁醇的N- [1-(氯甲基)丙基]亚氨代乙酰氯,其可以作为盐酸盐分离, 或游离碱或混合物,用L(+) - 酒石酸和d-2-氨基-1-丁醇分解,与二氯乙烷反应,然后与盐酸反应,形成乙胺丁醇盐酸盐。 方便分开的最少副产物允许经济地合成药物级产品。
    • 4. 发明授权
    • Process for preparing p-aminophenol and alkyl substituted p-aminophenol
    • 制备对氨基苯酚和烷基取代的对氨基苯酚的方法
    • US4415753A
    • 1983-11-15
    • US343993
    • 1982-01-29
    • Douglas C. CaskeyDouglas W. Chapman
    • Douglas C. CaskeyDouglas W. Chapman
    • C07B61/00B01J23/00C07C67/00C07C213/00C07C215/76C07C85/11C07C89/00
    • C07C215/76
    • A process for the production of unsubstituted and lower alkyl substituted p-aminophenols. A charge mixture is prepared comprising an unsubstituted or lower alkyl substituted nitrobenzene substrate, a platinum catalyst and a sulfur compound. The sulfur compound may be a divalent sulfur compound in which sulfur is bonded to two other moieties or a compound reducible to such sulfur compound under catalytic hydrogenation conditions. Hydrogen is introduced into the mixture while it is agitated at a temperature of 0.degree.-40.degree. C., thereby reducing the substrate to an unsubstituted or alkyl substituted phenylhydroxylamine. The hydroxylamine is thereafter heated to a temperature of at least 70.degree. C. and agitated at at least 70.degree. C. in the presence of a highly dissociated acid, thereby effecting rearrangement of the hydroxylamine to the corresponding p-aminophenol.
    • 一种制备未取代和低级烷基取代的对氨基苯酚的方法。 制备包含未取代或低级烷基取代的硝基苯底物,铂催化剂和硫化合物的电荷混合物。 硫化合物可以是二价硫化合物,其中硫在催化氢化条件下结合到两个其它部分或可还原成这种硫化合物的化合物。 将氢气在0℃-40℃的温度下搅拌引入混合物中,从而将底物还原成未取代或烷基取代的苯基羟胺。 然后将羟胺加热至至少70℃的温度,并在高度离解的酸存在下在至少70℃下搅拌,从而实现羟胺重排为相应的对氨基苯酚。