Weak acid process for producing dinitrotoluene
    22.
    发明授权
    Weak acid process for producing dinitrotoluene 失效
    弱酸工艺生产二硝基甲苯

    公开(公告)号:US5902910A

    公开(公告)日:1999-05-11

    申请号:US933706

    申请日:1997-09-19

    CPC classification number: C07C201/08

    Abstract: This invention relates to an improved process for the production of dinitrotoluene wherein one is able to effectively employ a feed sulfuric acid, which is referred to as "weak acid" as the feed sulfuric acid for the nitration facility. The weak acid concentration, as feed, ranges from 86-91%, preferably 87-89% sulfuric acid by weight, to meet the total sulfuric acid requirements for the facility. This is accomplished by utilizing cocurrent processing in a mononitration zone and countercurrent nitration with respect to sulfuric acid in the dinitration zone.

    Abstract translation: 本发明涉及生产二硝基甲苯的改进方法,其中能够有效地使用称为“弱酸”的进料硫酸作为硝化设备的进料硫酸。 作为进料的弱酸浓度范围为重量的86-91%,优选87-89%的硫酸,以满足该设施的总硫酸需求。 这是通过在单硝化区中使用并流处理和在二硝化区中相对于硫酸逆流硝化来实现的。

    Process for preparing 2-trifluoromethoxy-aniline
    23.
    发明授权
    Process for preparing 2-trifluoromethoxy-aniline 失效
    制备2-三氟甲氧基苯胺的方法

    公开(公告)号:US5840983A

    公开(公告)日:1998-11-24

    申请号:US896353

    申请日:1997-07-18

    CPC classification number: C07C205/37 C07C201/12 C07C213/02 C07C217/84

    Abstract: 2-Trifluoromethoxy-aniline, which can be used as an intermediate for example for preparing pharmaceuticals and agrochemicals, is obtained in very good yields and high purity by nitrating in a first step 1,2-dichlorotrifluoromethoxy-benzene at temperatures between -20.degree. C. and +80.degree. C. and catalytically hydrogenating the resulting nitration products (exclusively 1,2-dichloro-5-nitro-4-trifluoromethoxy-benzene and 1,2-dichloro-3-nitro-4-trifluoromethoxy-benzene) in a 2nd step, it being possible to isolate the aniline intermediates corresponding to the two nitrobenzene derivatives; the nitrobenzene and aniline derivatives mentioned, being novel compounds, are also part of the subject matter of the invention.

    Abstract translation: 可以用作制备药物和农业化学品的中间体的2-三氟甲氧基苯胺以非常好的产率和高纯度通过在第一步骤中通过在-20℃的温度下硝化来获得1,2-二氯三氟甲氧基 - 苯 和+ 80℃,并将所得硝化产物(仅1,2-二氯-5-硝基-4-三氟甲氧基 - 苯和1,2-二氯-3-硝基-4-三氟甲氧基 - 苯)催化氢化 第二步,可以分离对应于两种硝基苯衍生物的苯胺中间体; 提及的硝基苯和苯胺衍生物作为新化合物也是本发明主题的一部分。

    Process for the preparation of ethyl-N-(2,3 dichloro-6-nitrobenzyl)
glycine
    24.
    发明授权
    Process for the preparation of ethyl-N-(2,3 dichloro-6-nitrobenzyl) glycine 失效
    乙基-N-(2,3-二氯-6-硝基苄基)甘氨酸的制备方法

    公开(公告)号:US5801245A

    公开(公告)日:1998-09-01

    申请号:US919964

    申请日:1997-08-28

    Applicant: Philip C. Lang

    Inventor: Philip C. Lang

    Abstract: The known blood platelet reducing agent Anagrelide is prepared via an improved process starting with commercially available 2,3-dichlorotoluene and involving novel intermediates represented by the formulas: ##STR1## wherein Y is Br, Cl or I. Compound (G) is reacted with ethyl glycine to form the well-known intermediate ethyl-N-(2,3-dichloro-6-nitro benzyl) glycine which is then used following conventional process steps to form Anagrelide.

    Abstract translation: 已知的血小板减少剂阿那格雷通过改进的方法从市售的2,3-二氯甲苯开始制备,并涉及由下式表示的新型中间体:其中Y是Br,Cl 或I.化合物(G)与乙基甘氨酸反应以形成公知的中间体N-(2,3-二氯-6-硝基苄基)甘氨酸,然后按照常规方法步骤使用甘氨酸形成阿那格雷。

    Process for the production of 5-alkoxy-2,4-dinitro-alkylbenzenes
    25.
    发明授权
    Process for the production of 5-alkoxy-2,4-dinitro-alkylbenzenes 失效
    5-烷氧基-2,4-二硝基 - 烷基苯的制备方法

    公开(公告)号:US5382702A

    公开(公告)日:1995-01-17

    申请号:US142383

    申请日:1993-11-19

    CPC classification number: C07C201/08 C07C201/12

    Abstract: Process for producing 5-alkoxy-2,4-dinitroalkylbenzenes of the general formula (I) ##STR1## R.sup.1 =C.sub.1 to C.sub.4 alkyl; R=C.sub.1 to C.sub.6 alkyl group, C.sub.2 to C.sub.4 hydroxyalkyl, C.sub.3 to C.sub.4 dihydroxyalkyl,in which a 3-fluoroalkylbenzene is nitrated and the obtained 2,4-dinitro-5-fluoroalkylbenzene is then reacted with a suitable alcohol at -5.degree. C. to +25.degree. C. with the addition of sodium hydroxide or potassium hydroxide.

    Abstract translation: PCT No.PCT / EP93 / 00678 Sec。 371日期:1993年11月19日 102(e)1993年11月19日PCT 1993年3月20日PCT PCT。 出版物WO93 / 2551200 日本1993年12月23日。通式(I)的5-烷氧基-2,4-二硝基烷基苯的制备方法(Ⅰ)R1 = C1〜C4烷基; R = C1至C6烷基,C2至C4羟基烷基,C3至C4二羟基烷基,其中3-氟烷基苯被硝化,所得2,4-二硝基-5-氟烷基苯然后与适当的醇在-5℃下反应 至+ 25℃,加入氢氧化钠或氢氧化钾。

    One-step preparation of 4,6-dinitroresorcinol from resorcinol
    26.
    发明授权
    One-step preparation of 4,6-dinitroresorcinol from resorcinol 失效
    间苯二酚一步法制备4,6-二硝基间苯二酚

    公开(公告)号:US5371303A

    公开(公告)日:1994-12-06

    申请号:US213767

    申请日:1994-03-16

    CPC classification number: C07C201/08

    Abstract: 4,6-Dinitroresorcinol is prepared by reacting resorcinol with concentrated nitric acid that is substantially free of suboxides of nitric acid. It has been found that greater than 60 percent yields of the desired product can be obtained when the concentration of aqueous nitric acid used is between about 80 and about 93 weight percent, and the concentration of suboxides is less than about 2 weight percent based on the weight of nitric acid.

    Abstract translation: 通过使间苯二酚与基本上不含硝酸的低氧化物的浓硝酸反应来制备4,6-二硝基间苯二酚。 已经发现,当使用的硝酸水溶液的浓度为约80-约93重量%时,可以获得所需产物的大于60%的产率,并且低聚物的浓度小于约2重量%,基于 硝酸重量。

    Nitration process
    27.
    发明授权
    Nitration process 失效
    硝化过程

    公开(公告)号:US5313009A

    公开(公告)日:1994-05-17

    申请号:US135569

    申请日:1993-10-14

    Abstract: A continuous process to nitrate a nitratable aromatic compound in a nitronium ion solution in a nitrator. The process comprises feeding into the nitrator nitronium ion solution of a composition within an area defined by connecting three points in a ternary phase diagram of nitric acid, sulfuric acid and water. The three points correspond to first about 82% of sulfuric acid and 18% nitric acid, secondly about 55% sulfuric acid and about 45% water and, thirdly, 100% sulfuric acid, with the nitric acid preferably being below about 3%. The nitratable aromatic compound is introduced in a manner such that a fine emulsion of hydrocarbon in the nitronium ion solution is formed with the hydrocarbon evenly distributed in the acid phase. The acid and the nitratable aromatic compound are brought into intimate contact in a plug-flow nitrator that contains mixing elements.

    Abstract translation: 在氮化器中硝酸根离子溶液中硝化可硝化芳族化合物的连续方法。 该方法包括在硝酸,硫酸和水的三元相图中连接三个点所限定的区域内的组合物的硝化器硝鎓离子溶液中进料。 三点对应于首先约82%的硫酸和18%的硝酸,其次约55%的硫酸和约45%的水,以及第三种是100%的硫酸,硝酸优选低于3%左右。 引入可硝化芳族化合物,使得在硝酸根离子溶液中形成烃的精细乳液,其中均匀分布在酸相中的烃形成。 酸和可硝化芳香族化合物在包含混合元件的活塞式硝化器中紧密接触。

    Process for the preparation of 2-nitro-3, 6-dichlorophenol
    28.
    发明授权
    Process for the preparation of 2-nitro-3, 6-dichlorophenol 失效
    2-硝基-3,6-二氯苯酚的制备方法

    公开(公告)号:US5292966A

    公开(公告)日:1994-03-08

    申请号:US33110

    申请日:1993-03-16

    CPC classification number: C07C201/08

    Abstract: 2-Nitro-3,6-dichlorophenol is prepared by sulfonation of 2,5-dichlorophenol and subsequent nitration and desulfonation, in which the nitration is carried out by metering in a nitrating acid composed of 98 to 100% strength nitric acid and 96 to 100% strength sulfuric acid at temperatures from -15.degree. to 35.degree. C. and a metering time of at least 1 hour.

    Abstract translation: 2-硝基-3,6-二氯苯酚是通过2,5-二氯苯酚的磺化和随后的硝化和脱磺酸制备的,其中硝化是通过计量在由98至100%的强度硝酸组成的硝酸中进行的,而96- 在-15度至35摄氏度的温度下,100%强度的硫酸和至少1小时的计量时间。

    Process for preparing N-aliphatic substituted p-phenylenediamines
    29.
    发明授权
    Process for preparing N-aliphatic substituted p-phenylenediamines 失效
    制备N-脂族取代的对苯二胺的方法

    公开(公告)号:US5252737A

    公开(公告)日:1993-10-12

    申请号:US887981

    申请日:1992-05-22

    CPC classification number: C07C209/36 C07C209/02

    Abstract: A process for preparing N-aliphatic substituted p-phenylenediamine intermediates is provided which comprises contacting an aliphatic amine or substituted aliphatic amine derivative and nitrobenzene in the presence of a suitable solvent system, and reacting the aliphatic amine or substituted aliphatic amine derivative and nitrobenzene in the presence of a suitable base and a controlled amount of protic material at a suitable temperature in a confined reaction zone. In one embodiment, the N-aliphatic substituted p-phenylenediamine intermediates are reduced to N-aliphatic substituted p-phenylenediamines and the N-aliphatic substituted p-phenylenediamines can be reductively alkylated to N'-alkylated, N-aliphatic substituted p-phenylenediamines. In another embodiment of the invention, N-aliphatic substituted p-phenylenediamine intermediates are reductively alkylated to N'-alkylated, N-aliphatic substituted p-phenylenediamines.

    Abstract translation: 提供了一种制备N-脂族取代的对苯二胺中间体的方法,其包括在合适的溶剂体系的存在下使脂族胺或取代的脂族胺衍生物和硝基苯接触,并使脂族胺或取代的脂族胺衍生物和硝基苯在 在合适的温度下在约束反应区中存在合适的碱和受控量的质子物质。 在一个实施方案中,将N-脂族取代的对苯二胺中间体还原成N-脂族取代的对苯二胺,N-脂族取代的对苯二胺可以还原烷基化成N-烷基化的N-脂肪族取代的对苯二胺。 在本发明的另一个实施方案中,将N-脂族取代的对苯二胺中间体还原烷基化成N-烷基化的N-脂族取代的对苯二胺。

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