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61. 发明授权

US4454347A Process for purification and isolation of diaminophenylindane 失效
标题翻译：二氨基苯二氢茚的纯化和分离方法
公开(公告)号：US4454347A
公开(公告)日：1984-06-12
申请号：US465744
申请日：1983-02-11
申请人： Marc E. Parham , Stephen A. Spearman , Gleason O. Cookson
发明人： Marc E. Parham , Stephen A. Spearman , Gleason O. Cookson
IPC分类号： C07C209/86 , C07C67/00 , C07C209/00 , C07C211/45 , C07C211/54 , C07C85/26
CPC分类号： C07C209/84
摘要： Crystalline 5(6)-amino-1-(4-aminophenyl)-1,3,3-trimethylindane is made by crystallizing the diamino reaction mass from a toluene/heptane solution. The material has been previously purified through a combination of acetic acid washing and treatment with acidic clay. The diamino material, also known as DAPI, is a potential stabilizer, curing agent, and one of the monomers used to produce a polyimide resin.
摘要翻译：通过使二氨基反应物质从甲苯/庚烷溶液中结晶来制备结晶5（6） - 氨基-1-（4-氨基苯基）-1,3,3-三甲基茚满。先前通过乙酸洗涤和用酸性粘土处理的组合来纯化该物质。二氨基物质，也称为DAPI，是潜在的稳定剂，固化剂和用于生产聚酰亚胺树脂的单体之一。

62. 发明授权

US4416827A Process for the resolution of the racemate (1RS,2SR)-2-amino-1-phenyl-propan-1-ol 失效
标题翻译：拆分外消旋物（1RS，2SR）-2-氨基-1-苯基 - 丙-1-醇的方法
公开(公告)号：US4416827A
公开(公告)日：1983-11-22
申请号：US411325
申请日：1982-08-25
申请人： Horst Bethge , Axel Kleemann , Jurgen Martens
发明人： Horst Bethge , Axel Kleemann , Jurgen Martens
IPC分类号： C07B57/00 , C07B31/00 , C07C20060101 , C07C67/00 , C07C213/00 , C07C213/10 , C07C215/30 , C07C313/00 , C07C323/58 , C07C99/12 , C07C85/26
CPC分类号： C07C213/10 , C07C215/30 , C07C323/58 , C07B2200/07
摘要： There is described the resolution of the racemate (1RS,2SR)-2-amino-1-phenyl-propan-1-ol. It is carried out by means of the optical isomers of S-(carboxymethyl)-cysteine.
摘要翻译：描述了外消旋物（1RS，2SR）-2-氨基-1-苯基 - 丙-1-醇的拆分。它通过S-（羧甲基） - 半胱氨酸的光学异构体进行。

63. 发明授权

US4283254A Methylamines purification by distillation and purge 失效
标题翻译：通过蒸馏和吹扫纯化甲胺
公开(公告)号：US4283254A
公开(公告)日：1981-08-11
申请号：US136998
申请日：1980-04-03
申请人： Douglas E. Binau , Emmett J. Speicher
发明人： Douglas E. Binau , Emmett J. Speicher
IPC分类号： C07C211/04 , B01D3/14 , C07C67/00 , C07C209/00 , C07C85/26
CPC分类号： B01D3/14 , Y10S203/20
摘要： An improvement in the distillative refining of methylamines containing higher amine impurities wherein the higher amines accumulate in the distillation column, tending to cause flooding and product contamination. The improvement involves purging the column at the point the impurities concentrate, mixing the purge with water to form two phases, separating the phases and recycling the water phase for recovery of its methylamines content.
摘要翻译：改进含有较高胺杂质的甲胺的蒸馏精制，其中高级胺在蒸馏塔中积聚，倾向于引起淹水和产物污染。改进包括在杂质浓缩点清洗色谱柱，将清洗液与水混合以形成两相，分离各相并回收水相以回收其甲胺含量。

64. 发明授权

US4248798A New method for preparing pentanitroaniline and triaminotrinitrobenzenes from trinitrotoluene 失效
标题翻译：从三硝基甲苯制备戊基苯胺和三氨基硝基苯的新方法
公开(公告)号：US4248798A
公开(公告)日：1981-02-03
申请号：US116351
申请日：1980-01-28
申请人： Ronald L. Atkins , Arnold T. Nielsen , William P. Norris
发明人： Ronald L. Atkins , Arnold T. Nielsen , William P. Norris
IPC分类号： C06B25/04 , C07C85/00 , C07C85/02 , C07C85/11 , C07C85/26
CPC分类号： C06B25/04
摘要： Trinitrotoluene is selectively reduced by reaction with H.sub.2 S in p-dine to produce 4-amino-2,6-dinitrotoluene. This latter compound is then nitrated with HNO.sub.3 in H.sub.2 SO.sub.4 to produce pentanitroaniline which is, in turn, reacted with NH.sub.3 in benzene, methylene chloride or another suitable solvent to produce triaminotrinitrobenzene (TATB). TATB is useful as an explosive.
摘要翻译：通过与H 2 S在对二恶烷中反应选择性还原三硝基甲苯以产生4-氨基-2,6-二硝基甲苯。然后将后一种化合物用H 2 SO 4中的HNO 3硝化以产生戊基苯胺，其又在苯，二氯甲烷或其它合适的溶剂中与NH 3反应，产生三氨基硝基苯（TATB）。 TATB是有用的炸药。

65. 发明授权

US4224249A Toluene diamine from non-washed dinitrotoluene 失效
标题翻译：来自未洗涤二硝基甲苯的甲苯二胺
公开(公告)号：US4224249A
公开(公告)日：1980-09-23
申请号：US38976
申请日：1979-05-14
申请人： Nance D. Kunz , Thomas A. Johnson , Barton Milligan
发明人： Nance D. Kunz , Thomas A. Johnson , Barton Milligan
IPC分类号： C07B61/00 , B01J29/00 , C07C67/00 , C07C209/00 , C07C209/36 , C07C211/51 , C07C85/11 , C07C85/26
CPC分类号： C07C209/36
摘要： This invention relates to an improvement in a process for preparing toluene diamine. The improvement resides in a process which is capable of permitting reduction of dinitrotoluene to toluene diamine without prior alkaline treatment for removal of nitrocresols in the dinitrotoluene. In carrying out the improvement the feed dinitrotoluene is water washed to remove HNO.sub.3 to a level below 6000 ppm, and the catalytic conversion of dinitrotoluene to toluene diamine is done continuously. Dinitrotoluene is charged to a reaction vessel containing a liquid carrier and reduced with hydrogen at constant pressure, the dinitrotoluene being added at a rate to maintain a concentration of dinitrotoluene of 0.0001 to 25% by weight of the total reactor contents while the hydrogenation catalyst is maintained at a level from about 0.1 to 3% based on the weight of reactor contents.
摘要翻译：本发明涉及一种制备甲苯二胺的方法的改进。改进之处在于能够允许将二硝基甲苯还原成甲苯二胺而不经过碱性处理除去二硝基甲苯中的硝基甲酚。在进行改进时，将进料二硝基甲苯进行水洗以除去HNO 3至低于6000ppm的水平，并连续进行二硝基甲苯向甲苯二胺的催化转化。将二硝基甲苯加入到含有液体载体的反应容器中并在恒定压力下用氢气还原，二硝基甲苯的加入速率使二硝基甲苯的浓度保持在总反应器内容物的0.0001至25重量％，同时保持氢化催化剂基于反应器内容物的重量为约0.1至3％的水平。

66. 发明授权

US4217308A Process for preparing N-alkylethylenediamines 失效
标题翻译：制备N-烷基乙二胺的方法
公开(公告)号：US4217308A
公开(公告)日：1980-08-12
申请号：US48337
申请日：1979-06-14
申请人： Karel F. Bernady , Paul D. Mogolesko
发明人： Karel F. Bernady , Paul D. Mogolesko
IPC分类号： C07C209/08 , C07C85/04 , C07C85/26
CPC分类号： C07C209/08
摘要： This disclosure describes a novel process for preparing N-alkylethylenediamines which are useful as intermediates for purifying penicillins. N-alkylethylenediamines are also useful for preparing penicillins and cephalosporins. Specifically, N-ethylethylenediamine is useful for manufacturing piperacillin which is useful as an antibiotic.More particularly, the invention relates to a process for the efficient reaction of an alkyl halide and ethylenediamine and the recovery of anhydrous, ethylenediamine-free N-alkylethylenediamines therefrom.
摘要翻译：本公开描述了一种制备N-烷基亚乙二胺的新方法，其可用作纯化青霉素的中间体。 N-烷基乙二胺也可用于制备青霉素和头孢菌素。具体地说，N-乙基乙二胺可用于制备可用作抗生素的哌拉西林。更具体地说，本发明涉及一种烷基卤化物和乙二胺的有效反应和从其中回收无水，不含乙二胺的N-烷基乙二胺的方法。

67. 发明授权

US4201722A Process for separating 4,4'-diaminodiphenylmethane 失效
标题翻译：分离4,4'-二氨基二苯甲烷的方法
公开(公告)号：US4201722A
公开(公告)日：1980-05-06
申请号：US693081
申请日：1976-06-04
申请人： Kwok K. Sun
发明人： Kwok K. Sun
IPC分类号： C07C211/50 , C07C20060101 , C07C67/00 , C07C209/00 , C08G69/02 , C07C85/26
CPC分类号： C07C209/78
摘要： A process is described for the isolation of 4,4'-diaminodiphenylmethane in substantially pure form (of the order of 99% purity) from admixtures thereof with the corresponding 2,4'-isomer and 2,2'-isomer. The dihydrochloride of the isomeric mixture of diamines is heated in the presence of an inert organic solvent with a mixture of isomers of the free diamine, in which the amount of the 4,4'-isomer is at least equal to that of the 2,4'-isomer in the dihydrochloride isomeric mixture. The isomeric mixture of the diamines may be employed in the form of a mixture of polymethylene polyphenyl polyamines containing a major portion of said diamines. The reaction product consists of the insoluble dihydrochloride of substantially pure 4,4'-diaminodiphenylmethane and a solution which is enriched in 2,4'-isomer as compared with the starting mixture of diamines.
摘要翻译：描述了从其与相应的2,4'-异构体和2,2'-异构体的混合物分离基本上纯的形式（约99％纯度的）的4,4'-二氨基二苯基甲烷的方法。二胺的异构体混合物的二盐酸盐在惰性有机溶剂的存在下与游离二胺的异构体的混合物加热，其中4,4'-异构体的量至少等于2， 4'-异构体。二胺的异构体混合物可以以含有主要部分所述二胺的多亚甲基多苯基多胺的混合物的形式使用。反应产物由基本上纯的4,4'-二氨基二苯基甲烷的不溶性二盐酸盐和与二胺的起始混合物相比富含2,4'-异构体的溶液组成。

68. 发明授权

US4158016A Method for racemization of optically active amines 失效
标题翻译：光学活性胺外消旋化的方法
公开(公告)号：US4158016A
公开(公告)日：1979-06-12
申请号：US861515
申请日：1977-12-16
申请人： Tsuneyuki Nagase , Gohu Suzukamo , Yoshio Suzuki
发明人： Tsuneyuki Nagase , Gohu Suzukamo , Yoshio Suzuki
IPC分类号： C07B55/00 , C07C85/26
CPC分类号： C07B55/00
摘要： A method for racemization of optically active amines which comprises contacting an optically active amine of the formula: ##STR1## wherein C* is an asymmetric carbon atom, R.sub.1 is alkyl, aralkyl or aryl and R.sub.2 is aryl or alkoxycarbonyl, the aryl or aralkyl moiety bearing optionally one or more alkyl or alkoxy groups on the aromatic ring, provided that R.sub.1 and R.sub.2 are always different from each other, with a catalyst comprising an alkali metal and a polycyclic aromatic hydrocarbon until a sufficient amount of the optically active amine is racemized.
摘要翻译：一种光学活性胺外消旋化的方法，其包括使下式的光学活性胺：其中C *是不对称碳原子，R 1是烷基，芳烷基或芳基，R 2是芳基或烷氧基羰基，芳基或芳烷基部分如果R 1和R 2总是彼此不同，则在芳环上任选地具有一个或多个烷基或烷氧基，直到足够量的光学活性胺被外消旋化为止包含碱金属和多环芳烃的催化剂。

69. 发明授权

US4136118A Method of preparing 2,2'-dithiodianiline 失效
标题翻译：制备2,2“ - 二羟基苯胺的方法
公开(公告)号：US4136118A
公开(公告)日：1979-01-23
申请号：US826020
申请日：1977-08-19
申请人： Donald E. Smith , Charles B. Jones
发明人： Donald E. Smith , Charles B. Jones
IPC分类号： C07C319/20 , C07C20060101 , C07C67/00 , C07C313/00 , C07C319/14 , C07C323/33 , C07C323/37 , C07C85/24 , C07C85/26
CPC分类号： C07C319/24
摘要： Method of preparing 2,2'-dithiodianiline by the steps of (A) obtaining an agitated mixture of a water solution of a salt of o-aminothiophenol and an unstable dispersion therein of a liquid hydrocarbon, (B) oxidizing said salt by the slow addition of a water soluble peroxide, (C) discontinuing the agitation to allow the formation of a sharply defined lower aqueous phase and upper hydrocarbon phase, (D) drawing off said lower aqueous phase and (E) distilling the hydrocarbon phase therefrom and recovering said 2,2'-dithiodianiline as a distilland.
摘要翻译：通过（A）得到液体烃的邻氨基苯硫酚盐和其中不稳定分散体的水溶液的搅拌混合物的步骤（B），通过以下步骤制备2,2'-二硫代二苯胺的方法：（B）将缓慢加入水溶性过氧化物，（C）停止搅拌以形成明确限定的下部水相和上部烃相，（D）拉出所述下部水相，和（E）从其中蒸馏出烃相，回收所述的2,2'-二硫代二苯胺作为馏出物。

70. 发明授权

US4129580A Resolution of certain asymmetric primary amines using lasalocid 失效
标题翻译：使用拉沙洛尔的某些不对称伯胺的分辨率
公开(公告)号：US4129580A
公开(公告)日：1978-12-12
申请号：US851317
申请日：1977-11-14
申请人： John Westley
发明人： John Westley
IPC分类号： C07D307/22 , C07C85/26
CPC分类号： C07D307/22
摘要： Racemic modifications of optically active primary or tertiary amines are treated with lasalocid to form diastereomeric salts. The so-formed diastereomeric salts are separated and, subsequently, can be chemically decomposed to give the desired enantiomers of the amine. The resolving agent, lasalocid, is recovered in this process by precipitation or evaporation from organic solvents.
摘要翻译：光学活性伯或仲胺的外消旋体改性用拉沙里菌素处理以形成非对映体盐。将如此形成的非对映异构体盐分离，随后可以化学分解，得到胺的所需对映异构体。通过沉淀或蒸发有机溶剂，在该方法中回收拆分剂拉沙洛尔。

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