Process for the preparation of 4,6-diaminoresorcinol
    21.
    发明授权
    Process for the preparation of 4,6-diaminoresorcinol 失效
    制备4,6-二氨基间苯二酚的方法

    公开(公告)号:US5574188A

    公开(公告)日:1996-11-12

    申请号:US549241

    申请日:1995-10-27

    摘要: 4,6-diaminoresorcinol can be prepared in a plurality of steps in such a way thata) 1,3-dichlorobenzene is nitrated with a mixed acid of HNO.sub.3, H.sub.2 SO.sub.4 and SO.sub.3 at 0 to 40.degree. C. in anhydrous H.sub.2 SO.sub.4,b) the resulting 1,3-dichloro-4,6/2,4-dinitrobenzene isomeric mixture is first reacted with benzyl alcohol in the presence of a strong base at -15.degree. C. to +15.degree. C. and then at 20.degree. to 40.degree. C. to give the dibenzyloxy compound andc) the 1,3-dibenzyloxy-4,6-dinitrobenzene isomer arising in pure form in b) is converted to the 4,6-diaminoresorcinol by catalytic hydrogenation.

    摘要翻译: 可以以多个步骤制备4,6-二氨基间苯二酚,使得a)在无水H 2 SO 4中在0至40℃下用HNO 3,H 2 SO 4和SO 3的混合酸硝化1,3-二氯苯,b) 所得的1,3-二氯-4,6 / 2,4-二硝基苯异构体混合物首先在强碱存在下在-15℃至+ 15℃下与苄醇反应,然后在20℃至 40℃,得到二苄氧基化合物,和c)在b)中以纯形式产生的1,3-二苄氧基-4,6-二硝基苯异构体通过催化氢化转化为4,6-二氨基间苯二酚。

    Process for the isolation of 1-naphthylamine-4,8-disulphonic acid
    24.
    发明授权
    Process for the isolation of 1-naphthylamine-4,8-disulphonic acid 失效
    分离1-萘胺-4,8-​​二磺酸的方法

    公开(公告)号:US4407762A

    公开(公告)日:1983-10-04

    申请号:US410746

    申请日:1982-08-23

    CPC分类号: C07C303/44

    摘要: Process for the isolation of 1-naphthylamine-4,8-disulphonic acid from sulphonation mixtures containing it according to which process the sulphonation mixture is introduced into preheated water in such a manner that, at the start of crystallization, a temperature of at least 100.degree. C. is reached and the 1-naphthylamine-4,8-disulphonic acid is separated from the mother liquor at a temperature not higher than 70.degree. C. The process is applied particularly advantageously for the isolation of 1-naphthylamine-4,8-disulphonic acid from sulphonation mixtures which have been obtained by introducing in turns alkali metal sulphate, 1-naphthylamine-8-sulphonic acid and SO.sub.3 into sulphuric acid which has been introduced initially, a total of 1.5 to 3 mols of SO.sub.3 and 0.6 to 1.5 mols of alkali metal sulphate being employed per mol of 1-naphthylamine-8-sulphonic acid.

    摘要翻译: 从含有它的磺化混合物中分离出1-萘胺-4,8-​​二磺酸的方法,根据该方法,将磺化混合物引入预热的水中,使得在结晶开始时,温度至少为100 达到C,并且在不高于70℃的温度下将1-萘胺-4,8-​​二磺酸与母液分离。该方法特别有利地用于分离1-萘胺-4,8 来自磺化混合物的二磺酸通过将碱金属硫酸盐,1-萘胺-8-磺酸和SO 3引入到最初引入的硫酸中,总共含有1.5至3摩尔的SO 3和0.6至1.5 每摩尔1-萘胺-8-磺酸使用碱金属硫酸盐的摩尔数。

    Process for the preparation of naphthalene-1,3,5-trisulphonic acid
    25.
    发明授权
    Process for the preparation of naphthalene-1,3,5-trisulphonic acid 失效
    制备萘-1,3,5-三磺酸的方法

    公开(公告)号:US4369143A

    公开(公告)日:1983-01-18

    申请号:US287591

    申请日:1981-07-28

    CPC分类号: C07C309/00

    摘要: A process is provided for the preparation of naphthalene-1,3-5,-trisulphonic acid from 1,5-disulphonated naphthalene, which comprises sulphonating 1,5-disulphonated naphthalene, in the form of a mixture which has been obtained by mixing naphthalene and SO.sub.3 in the presence of an inert solvent at temperatures in the range of -40.degree. to +20.degree. C., the ratio of SO.sub.3 added to naphthalene added having been in the range of 2.5 to 10 mols of SO.sub.3 per mol of naphthalene during the entire addition, at 60.degree. to 110.degree. C. in anhydrous sulphuric acid with oleum, with prior or concurrent separation of the inert solvent.The resulting product is a known intermediate for the formation of azo dyestuffs.

    摘要翻译: 提供了从1,5-二磺酸萘制备萘-1,3,5-三磺酸的方法,该方法包括将1,5-二磺酸萘磺化为混合物形式,其通过将萘 和SO 3在惰性溶剂存在下,在-40℃至+ 20℃的温度范围内,加入的萘的添加比例在2.5至10摩尔的SO 3 /摩尔萘的范围内 全部加入,在60〜110℃下用无水硫酸与发烟硫酸,先后或同时分离惰性溶剂。 所得产物是用于形成偶氮染料的已知中间体。

    Process for the isolation of 1-naphthylamine-4,6- and
1-naphthylamine-4,7-disulphonic acid
    26.
    发明授权
    Process for the isolation of 1-naphthylamine-4,6- and 1-naphthylamine-4,7-disulphonic acid 失效
    分离1-萘胺-4,6-和1-萘胺-4,7-二磺酸的方法

    公开(公告)号:US4348336A

    公开(公告)日:1982-09-07

    申请号:US247414

    申请日:1981-03-25

    CPC分类号: C07C303/06

    摘要: Process for the isolation of 1-naphthylamine-4,6- or 1-naphthylamine-4,7-disulphonic acid from sulphonation mixtures obtained in the sulphonation of 1-naphthylamine-6- or 1-naphthylamine-7-sulphonic acid with sulphuric acid and sulphur trioxide, wherein the aqueous solutions or suspensions formed, when the sulphonation mixtures are introduced into water, are warmed to 80.degree. to 120.degree. C., optionally kept for a period of time at this temperature, are then cooled to temperatures below 70.degree. C., and the 1-naphthylamine-4,6- or 1-naphthylamine-4,7-disulphonic acid which has crystallized out is finally filtered off.

    摘要翻译: 从1-萘胺-6-或1-萘胺-7-磺酸与硫酸磺化得到的磺化混合物中分离1-萘胺-4,6-或1-萘胺-4,7-二磺酸的方法 和三氧化硫,其中当将磺化混合物引入水中时形成的水溶液或悬浮液被加热至80℃至120℃,任选地在该温度下保持一段时间,然后冷却至低于70℃ 并结晶出的1-萘胺-4,6-或1-萘胺-4,7-二磺酸终于被滤出。

    Process for the preparation of 1,5-dihydroxynaphthalene and
1,5-diaminonaphthalene
    30.
    发明授权
    Process for the preparation of 1,5-dihydroxynaphthalene and 1,5-diaminonaphthalene 失效
    制备1,5-二羟基萘和1,5-二氨基萘的方法

    公开(公告)号:US4973758A

    公开(公告)日:1990-11-27

    申请号:US439757

    申请日:1989-11-21

    摘要: The characteristic of the improved process for the preparation of 1,5-dihydroxynaphthalene and 1,5-diaminonaphthalene is to carry out the alkaline pressure hydrolysis of the disodium salt of naphthalene-1,5-disulphonic acid at temperatures from 270.degree. to 290.degree. C. and under 14 to 20 bar using an excess of sodium hydroxide solution such that the molar ratio NaOH/disodium salt of naphthalenesulphonic acid is at least 12:1. The 1,5-dihydroxynaphthalene which is obtained in this manner, without hazard and in substantially higher purity, is then aminated with ammonia in the presence of ammonium bisulphite to give 1,5-diaminonaphthalene, it being possible to achieve a further increase in the degree of purity of the 1,5-diaminonaphthalene by increasing the molar ratio NH.sub.3 /1,5-dihydroxynaphthalene to at least 6:1.

    摘要翻译: 制备1,5-二羟基萘和1,5-二氨基萘的改进方法的特点是在270〜290℃的温度下进行萘-1,5-二磺酸二钠盐的碱性水解 并使用过量的氢氧化钠溶液使14至20巴,使得萘磺酸的NaOH /二钠盐的摩尔比至少为12:1。 然后用亚硫酸铵存在下用氨将胺化得到的1,5-二羟基萘没有危害并且纯度高得多,得到1,5-二氨基萘,可以进一步增加 通过将NH 3 / 1,5-二羟基萘的摩尔比提高到至少6:1,1,5-二氨基萘的纯度。