Process for the preparation of naphthalene-1,3,6-trisulphonic acid
    1.
    发明授权
    Process for the preparation of naphthalene-1,3,6-trisulphonic acid 失效
    制备萘-1,3,6-三磺酸的方法

    公开(公告)号:US4180521A

    公开(公告)日:1979-12-25

    申请号:US886696

    申请日:1978-03-15

    CPC分类号: C07C309/00

    摘要: A process has been invented for the preparation of naphthalene-1,3,6-trisulphonic acid by sulphonating naphthalene with sulphuric acid and oleum, characterized in that naphthalene and most of the oleum are simultaneously metered into sulphuric acid or oleum of low concentration, which has been initially introduced, at about 140.degree. to 240.degree. C., the temperature is kept at about 140.degree. to 240.degree. C. for some time, the remainder of the oleum is then added at about 140.degree. to 240.degree. C. and the mixture is then further stirred for some time.Naphthalene-1,3,6-trisulphonic acid is a known important intermediate used, for example, in the preparation of T-acid, H-acid and chromotropic acid.

    摘要翻译: 已经发明了通过用硫酸和发烟硫酸磺化萘来制备萘-1,3,6-三磺酸的方法,其特征在于萘和大多数发烟硫酸同时计量成低浓度的硫酸或发烟硫酸,其中 最初在约140℃至240℃下引入,温度保持在约140℃至240℃一段时间,然后在约140℃至240℃加入发烟硫酸的其余部分, 然后将混合物进一步搅拌一段时间。 萘-1,3,6-三磺酸是已知的重要中间体,例如用于制备T酸,H酸和变色酸。

    Process for producing the magnesium salt of
3-nitro-naphthalene-1,5-disulfonic acid (nitro-Armstrong's acid)
    2.
    发明授权
    Process for producing the magnesium salt of 3-nitro-naphthalene-1,5-disulfonic acid (nitro-Armstrong's acid) 失效
    制备3-硝基 - 萘-1,5-二磺酸镁盐(硝基 - 阿姆斯壮酸)的方法

    公开(公告)号:US4348334A

    公开(公告)日:1982-09-07

    申请号:US113412

    申请日:1980-01-18

    CPC分类号: C07C309/00

    摘要: A process for producing the magnesium salt of 3-nitro-naphthalene-1,5-disulfonic acid by sulfonating naphthalene, nitrating the sulfonation product, and separating the pure magnesium salt of 3-nitronaphthalene-1,5-disulfonic acid, which process comprises:(a) sulfonating naphthalene with liquid SO.sub.3 in the presence of an inert organic solvent at temperatures between -40.degree. and +20.degree. C.;(b) adding to the reaction mixture obtained a mixture consisting of about equal parts of 100% sulfuric acid and fully reacted crude nitration mixture from nitration of a previous nitration charge, separating from the resulting two-phase system the upper organic solvent phase by decanting, and removing from the Armstrong's acid anhydride acid slurry the remainder of organic solvent by distillation, or removing it during or after subsequent nitration, subsequently adding to the residue the amount of nitric acid required for nitration, and then nitrating;(c) adding then firstly water and afterwards, in the absence of the inert organic solvent, at 90.degree. to 120.degree. C., a compound releasing magnesium ions, the amount being such that, per mol of 3-nitronaphthalene-1,5-disulfonic acid, 1.1 to 1.3 mols of magnesium ions are added, and a sulfuric acid concentration of between 40 and 60 percent by weight (relative to the sulfuric acid and water) is maintained; and(d) separating the crystallized magnesium salt of 3-nitronaphthalene-1,5-disulfonic acid at a temperature of between 20.degree. and 70.degree. C., and subsequently optionally washing it with a maximum of 60 percent by weight of sulfuric acid and/or water, and optionally drying the product.

    摘要翻译: 通过磺化萘,硝化磺化产物和分离3-硝基萘-1,5-二磺酸的纯镁盐来生产3-硝基 - 萘-1,5-二磺酸的镁盐的方法,该方法包括 :(a)在-40℃〜+ 20℃的温度下,在惰性有机溶剂的存在下,用液态SO 3磺化萘。 (b)向反应混合物中加入由约等量的100%硫酸组成的混合物和来自先前硝化装置的硝化的完全反应的粗硝化混合物,通过倾析从所得两相体系中分离出上部有机溶剂相 ,并通过蒸馏从阿姆斯壮的酸酐酸浆中除去剩余的有机溶剂,或者在后续硝化过程中或之后将其除去,随后向残余物中加入硝化所需的硝酸量,然后硝化; (c)然后首先加入水,然后在不存在惰性有机溶剂的情况下,在90〜120℃下,加入释放镁离子的化合物,其用量为每摩尔3-硝基萘-1,5 二磺酸,加入1.1〜1.3摩尔的镁离子,硫酸浓度保持在40〜60重量%之间(相对于硫酸和水); 和(d)在20℃至70℃的温度下分离3-硝基萘-1,5-二磺酸的结晶镁盐,随后任选地用最多60重量%的硫酸洗涤, /或水,并任选地干燥产品。

    Process for the preparation of 1-amino-8-naphthol-3,6-disulphonic acid
(H-acid)
    5.
    发明授权
    Process for the preparation of 1-amino-8-naphthol-3,6-disulphonic acid (H-acid) 失效
    制备1-氨基-8-萘酚-3,6-二磺酸(H酸)的方法

    公开(公告)号:US4325889A

    公开(公告)日:1982-04-20

    申请号:US186884

    申请日:1980-09-12

    IPC分类号: C07C143/66

    摘要: The invention relates to a process for the preparation of 1-amino-8-naphthol-3,6-disulphonic acid (H-acid) as the mono-alkali metal salt from napthylamine-trisulphonic acid isomer mixtures by alkaline hydrolysis under pressure. The separation of the H-acid is effected by utilizing an aqueous sulphuric acid which contains naphthalene- and/or nitronaphthalene- and/or naphthylamine- and/or naphthol- and/or aminonaphthol-mono-, -di-and/or-tri-sulphonic acids.

    摘要翻译: 本发明涉及通过碱性水解在压力下从萘胺 - 三磺酸异构体混合物制备作为单碱金属盐的1-氨基-8-萘酚-3,6-二磺酸(H-酸)的方法。 H酸的分离是通过利用含有萘和/或硝基萘和/或萘胺和/或萘酚和/或氨基萘酚 - 单 - 和 - 或 - 三 - 磺酸。

    Method for producing 4,6-dichloropyrimidine with sulfur compounds and phosphorus compounds
    6.
    发明授权
    Method for producing 4,6-dichloropyrimidine with sulfur compounds and phosphorus compounds 失效
    用硫化合物和磷化合物生产4,6-二氯嘧啶的方法

    公开(公告)号:US06525198B1

    公开(公告)日:2003-02-25

    申请号:US10069089

    申请日:2002-02-07

    IPC分类号: C07D23930

    CPC分类号: C07D239/30

    摘要: The invention relates to a method for the preparation of 4,6-dichloropyrimidine by reacting 4-chloro-6-methoxypyrimidine with at least one sulphur-containing chlorinating agent selected from the group consisting of SCl2, SOCl2, and SO2Cl2 in the presence of at least one phosphorus compound having the formula R3P═Yn  (1), in which R represents C1-C10-alkyl or C6-C10-aryl, each of which may optionally be substituted by up to five identical or different substituents selected from the group consisting of fluorine, chlorine, bromine, C1-C4-alkyl, and C1-C4-alkoxy, Y represents oxygen or sulphur, and n represents zero or 1.

    摘要翻译: 本发明涉及通过使4-氯-6-甲氧基嘧啶与至少一种选自SCl 2,SOCl 2和SO 2 Cl 2的含硫氯化剂在存在下进行反应来制备4,6-二氯嘧啶的方法 至少一种具有式(I)的磷化合物,其中R表示C 1 -C 10 - 烷基或C 6 -C 10 - 芳基,其各自可任选被至多五个相同或不同的选自氟,氯,溴,C1- C 4 - 烷基和C 1 -C 4 - 烷氧基,Y表示氧或硫,并且n表示0或1。

    Method of preparing 4,5,6-trichloro- and 2,4,5,6-tetrachloropyrimidine
    7.
    发明授权
    Method of preparing 4,5,6-trichloro- and 2,4,5,6-tetrachloropyrimidine 失效
    制备4,5,6-三氯 - 和2,4,5,6-四氯嘧啶的方法

    公开(公告)号:US6162917A

    公开(公告)日:2000-12-19

    申请号:US194983

    申请日:1998-12-07

    IPC分类号: C07C255/24 C07D239/30

    CPC分类号: C07D239/30 C07C255/24

    摘要: The invention relates to a process for the preparation of 4,5,6-trichloro- and 2,4,5,6-tetrachloropyrimidine starting from 3-dimethylamino-propionitrile, to its use and also to a crystalline intermediate product form.

    摘要翻译: PCT No.PCT / EP97 / 02933 371日期1998年12月7日第 102(e)日期1998年12月7日PCT提交1997年6月6日PCT公布。 公开号WO97 / 47605 日期:1997年12月18日本发明涉及从3-二甲基氨基 - 丙腈开始制备4,5,6-三氯 - 和2,4,5,6-四氯嘧啶的方法,其用途和结晶中间体 产品形式。

    Process for the preparation of 2-chloroacrylonitrile
    8.
    发明授权
    Process for the preparation of 2-chloroacrylonitrile 失效
    制备2-氯丙烯腈的方法

    公开(公告)号:US5679826A

    公开(公告)日:1997-10-21

    申请号:US735717

    申请日:1996-10-23

    CPC分类号: C07C253/30

    摘要: 2-Chloroacrylonitrile is prepared in a particularly advantageous and readily industrially practicable manner by chlorinating acrylonitrile and then thermally cleaving the 2,3-diehloropropionitrile formed, by chlorinating acrylonitrile in the presence of a catalyst system comprising dimethylformamide and pyridine and/or pyridine derivatives and subjecting the resulting crude 2,3-dichloropropionitrile to thermal cleavage in the presence of the same catalyst system without the addition of further catalysts.

    摘要翻译: 通过氯化丙烯腈,然后在包含二甲基甲酰胺和吡啶和/或吡啶衍生物的催化剂体系存在下,通过氯化丙烯腈热分解形成的2,3-二氯丙腈,制备2-氯丙烯腈, 所得粗制的2,3-二氯丙腈在相同的催化剂体系的存在下进行热裂解而不加入另外的催化剂。

    Process for the preparation of Grignard reagents and novel Grignard reagents
    10.
    发明授权
    Process for the preparation of Grignard reagents and novel Grignard reagents 失效
    格氏试剂和新型格氏试剂的制备方法

    公开(公告)号:US06296788B1

    公开(公告)日:2001-10-02

    申请号:US09615434

    申请日:2000-07-13

    IPC分类号: C07F302

    CPC分类号: C07F3/02

    摘要: Grignard reagents which contain a protected aldehyde function are obtained in a particularly advantageous manner from a halogenated aldehyde by reaction with a secondary monoamine to give an open-chain aminal, and conversion of the latter into a Grignard reagent using metallic magnesium. The invention also relates to novel Grignard reagents of this type.

    摘要翻译: 通过与二级单胺反应,以卤代醛特别有利的方式得到含有保护的醛官能团的格氏试剂,得到开链的氨基甲酸酯,并使用金属镁将其转化成格氏试剂。 本发明还涉及这种类型的新型格氏试剂。