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    • 6. 发明授权
    • Purification of 2-nitro-4-methylsulphonylbenzoic acid
    • 2-硝基-4-甲基磺酰基苯甲酸的纯化
    • US07285678B2
    • 2007-10-23
    • US10472962
    • 2002-03-25
    • Kambiz JavdaniGilbert RodriguezJames Peter Muxworthy
    • Kambiz JavdaniGilbert RodriguezJames Peter Muxworthy
    • C07C315/06
    • C07C315/06C07C317/44
    • A method for removing impurities from 2-nitro-4-methylsulfonylbenzoic acid which comprises at least two of the following steps, in any order, (a) dissolving 2-nitro-4-methylsulfonylbenzoic acid in water at a pH of about 2 to 10, followed by filtration; (b) contacting an aqueous solution of 2-nitro-4-methylsulfonylbenizoic acid with activated carbon at a pH of about 2 to 10; (c) treating an aqueous solution of 2-nitro-4-methylsulfonylbenzoic acid with sufficient base to hydrolyze undesired nitro and dinitro substituted impurities; followed by maintaining the resulting aqueous solution comprising 2-nitro-4-methylsulfonylbenzoic acid at a temperature of up to about 95° C., and adjusting the pH of said solution to about a pH which is sufficient to effect crystallization of 2-nitro-4-methylsulfonylbenzoic acid upon cooling.
    • 一种从2-硝基-4-甲基磺酰基苯甲酸中除去杂质的方法,该方法包括至少两个以下步骤,以任何顺序,(a)将2-硝基-4-甲基磺酰基苯甲酸溶于约2至10的pH下的水中 ,然后过滤; (b)将2-硝基-4-甲基磺酰基二十八碳酸的水溶液与约2至10的pH下的活性炭接触; (c)用足够的碱处理2-硝基-4-甲基磺酰基苯甲酸的水溶液以水解不希望的硝基和二硝基取代的杂质; 然后将所得到的包含2-硝基-4-甲基磺酰基苯甲酸的水溶液在高至约95℃的温度下保持,并将所述溶液的pH调节至足以使2-硝基-4-甲基磺酰基苯甲酸结晶的pH值, 4-甲基磺酰基苯甲酸。
    • 9. 发明授权
    • Process for the nitration of diphenylethers
    • 硝基二苯醚的工艺
    • US6028219A
    • 2000-02-22
    • US901545
    • 1997-07-28
    • John Heathcote AthertonStephen Martin BrownJames Peter MuxworthyMartin Lennon
    • John Heathcote AthertonStephen Martin BrownJames Peter MuxworthyMartin Lennon
    • C07B43/02C07C201/08C07C205/38C07C205/59C07C205/60C07C303/40C07C311/51C07C205/06
    • C07C201/08C07C303/40
    • A process for the preparation of a compound of general formula I: ##STR1## wherein: R.sup.1 is hydrogen or C.sub.1 -C.sub.6 alkyl, C.sub.2 -C.sub.6 alkenyl or C.sub.2 -C.sub.6 alkynyl, any of which may optionally be substituted with one or more substituents selected from halogen and OH; or COOR.sup.4, COR.sup.6, CONR.sup.4 R.sup.5 or CONHSO.sub.2 R.sup.4 ;R.sup.4 and R.sup.5 are each independently hydrogen or C.sub.1 -C.sub.4 alkyl optionally substituted with one or more halogen atoms;R.sup.6 is a halogen atom or a group R.sup.4 ;R.sup.2 is hydrogen or halo;R.sup.3 is C.sub.1 -C.sub.4 alkyl, C.sub.2 -C.sub.4 alkenyl or C.sub.2 -C.sub.4 alkynyl, any of which may optionally be substituted with one or more halogen atoms; or halo;the process comprising reacting a compound of general formula II: ##STR2## wherein R.sup.1, R.sup.2 and R.sup.3 are as defined for general formula I; with a nitrating agent comprising nitric acid or a mixture of nitric and sulphuric acids in the presence of an organic solvent and in the presence of acetic anhydride, characterized in that the molar ratio of acetic anhydride to compound of general formula II is from about 1:1 to 3:1.
    • 一种制备通式I化合物的方法:其中:R 1是氢或C 1 -C 6烷基,C 2 -C 6烯基或C 2 -C 6炔基,其中任何一个可以被一个或多个选自卤素和 哦; 或COOR4,COR6,CONR4R5或CONHSO2R4; R 4和R 5各自独立地为氢或任选被一个或多个卤素原子取代的C 1 -C 4烷基; R6是卤素原子或基团R4; R2是氢或卤素; R 3是C 1 -C 4烷基,C 2 -C 4烯基或C 2 -C 4炔基,其中任何一个可以任选被一个或多个卤素原子取代; 或卤素; 所述方法包括使通式II的化合物:其中R 1,R 2和R 3如通式I所定义; 与硝酸和硝酸和硫酸的混合物在有机溶剂的存在下和在乙酸酐存在下的硝化剂,其特征在于乙酸酐与通式II的化合物的摩尔比为约1: 1到3:1。