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1. 发明授权

US4338473A Method for removing nitrosation agent(s) from a nitrated aromatic compound 失效
标题翻译：从硝化芳族化合物中除去亚硝化剂的方法
公开(公告)号：US4338473A
公开(公告)日：1982-07-06
申请号：US151286
申请日：1980-05-19
申请人： Kurt Habig , Konrad Baessler , Lothar Schulz , Heinz Schutte
发明人： Kurt Habig , Konrad Baessler , Lothar Schulz , Heinz Schutte
IPC分类号： C07B43/02 , C07C201/16 , C07C76/02 , C07C79/10 , C07C79/12
CPC分类号： C07C201/16 , C07B43/02
摘要： Nitrosation agent(s), contained as by-products in nitrated aromatic compounds after nitration with nitric acid or nitration acid, are removed by a water treatment, wherein the water is distilled off at least partially in vapor form, advantageously under reduced pressure. In the further reaction of the nitrocompounds treated in this manner undesired nitrosamines are practically not formed. The process is especially suitable for the manufacture of 4-di-n-propylamino-3,5-dinitrobenzotrifluoride (Trifluralin), a valuable herbicide, substantially free from nitrosamine(s).
摘要翻译：通过水处理除去在用硝酸或硝酸酸硝化之后在硝化芳族化合物中作为副产物包含的亚硝化剂，其中有利地在减压下至少部分地以蒸气形式蒸馏掉水。在以这种方式处理的硝基化合物的进一步反应中，实际上不形成不希望的亚硝胺。该方法特别适用于生产基本上不含亚硝胺的有价值的除草剂4-二正丙基氨基-3,5-二硝基三氟甲苯（Trifluralin）。

2. 发明授权

US5208376A Process for the continuous preparation of 3,3'-dichloro-benzidine dihydrochloride 失效
标题翻译：连续制备3,3'-二氯苯胺二氯化物的方法
公开(公告)号：US5208376A
公开(公告)日：1993-05-04
申请号：US856063
申请日：1992-06-08
申请人： Kurt Habig , Konrad Baessler , Klaus Warning
发明人： Kurt Habig , Konrad Baessler , Klaus Warning
IPC分类号： C07C209/42 , C07C209/54 , C07C211/52
CPC分类号： C07C209/54
摘要： A process for the continuous preparation of 3,3'-dichlorobenzidine dihydrochloride from 2,2'-dichlorohydrazobenzene by treatment with aqueous sulfuric acid, which comprises treating the 2,2'-dichlorohydrazobenzene, dissolved in a water-immiscible aromatic solvent, continuously at temperatures of from about 20.degree. to about 50.degree. C. in the presence of an alkali metal salt of an alkyl (C.sub.8 -C.sub.23)polyglycol ether sulfate, with such an amount of from about 50 to about 80 % strength aqueous sulfuric acid that the suspension formed remains conveyable, subsequently diluting the suspension emerging from the reaction zone with water, again continuously, and subsequently heating the suspension to a temperature of from about 90.degree. to about 95.degree. C. until a solution is obtained, separating off the aromatic solvent from the hot, sulfuric acid aqueous phase, and precipitating the 3,3'-dichlorobenzidine dihydrochloride by adding hydrochloric acid to the sulfuric acid solution which remains and filtering off this product.
摘要翻译： PCT No.PCT / EP90 / 01844 Sec。 371日期：1992年6月8日 102（e）日期1992年6月8日PCT 1990年11月3日PCT PCT。第WO91 / 07377号公报日本1991年5月30日。一种通过用硫酸水溶液连续制备3,3'-二氯联苯胺二盐酸盐的方法，该方法包括处理溶于水中的2,2'-二氯代苯，不饱和的芳族溶剂，在约20至约50℃的温度下，在烷基（C 8 -C 23）聚乙二醇醚硫酸盐的碱金属盐存在下，其量为约50至约80％形成的悬浮液的强度硫酸水溶液仍然是可输送的，随后再次用水稀释从反应区出来的悬浮液，随后将悬浮液加热到约90℃至约95℃的温度，直至获得溶液，从热硫酸水相中分离芳族溶剂，并通过向硫酸溶液中加入盐酸沉淀出3,3'-二氯联苯胺二盐酸盐，其中r 发出并过滤掉本产品。

3. 发明授权

US5041671A Process for the preparation 4-chloro-2,5-dimethoxy-aniline 失效
标题翻译： 4-氯-2,5-二甲氧基苯胺的制备方法
公开(公告)号：US5041671A
公开(公告)日：1991-08-20
申请号：US369290
申请日：1989-06-21
申请人： Klaus Warning , Kurt Habig
发明人： Klaus Warning , Kurt Habig
IPC分类号： B01J23/42 , C07B61/00 , C07C213/02 , C07C217/84
CPC分类号： C07C213/02
摘要： Process for the preparation of 4-chloro-2,5-dimethoxyaniline by catalytic reduction of 4-chloro-2,5-dimethoxynitrobenzene with hydrogen in the liquid phase at an elevated temperature and elevated pressure, which comprises carrying out the reduction at temperatures from about 80.degree. to about 110.degree. C. and under a pressure of about 5 to 50 atmospheres gauge in an aromatic solvent in the presence of a modified platinum-on-carbon catalyst in the presence of about 0.01 to about 0.2 mole of a compound which gives a pH of 8 to 10 in aqueous solution, and in the presence of about 0.1 to about 1.0% by weight of an aliphatic, open-chain, primary, secondary or tertiary amine or a cyclic amine, in each case relative to the amount in moles and weight, respectively, of 4-chloro-2,5-dimethoxynitrobenzene employed.
摘要翻译：通过在高温和高压下在液相中用氢气还原4-氯-2,5-二甲氧基硝基苯来制备4-氯-2,5-二甲氧基苯胺的方法，其包括在在约0.01至约0.2摩尔的化合物存在下，在芳族溶剂中，在改性的铂 - 碳催化剂的存在下，在约0.1-约0.2摩尔的化合物存在下，在约5-约50℃的压力下，在水溶液中提供8至10的pH，并且在约0.1至约1.0重量％的脂族，开链，伯，仲或叔胺或环胺的存在下，在每种情况下相对于分别为使用的4-氯-2,5-二甲氧基硝基苯的摩尔数和重量。

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