公开(公告)号：US5910604A

公开(公告)日：1999-06-08

申请号：US816930

申请日：1997-03-13

Applicant: Stephen Martin Brown ,  Brian David Gott ,  Thomas Gray ,  Seyed Mehdi Tavana

Inventor： Stephen Martin Brown ,  Brian David Gott ,  Thomas Gray ,  Seyed Mehdi Tavana

IPC: C07C201/16 ,  C07C205/59 ,  C07C303/36 ,  C07C303/44 ,  C07C311/51

CPC classification number: C07C303/44 ,  C07C201/16

Abstract: A process for the purification of a compound of general formula I: ##STR1## wherein R.sup.1 is hydrogen or C.sub.1 -C.sub.6 alkyl, C.sub.2 -C.sub.6 alkenyl or C.sub.2 -C.sub.6 alkynyl, any of which may optionally be substituted with one or more substituents selected from halogen and hydroxy; or COOR.sup.4, COR.sup.6, CONR.sup.4 R.sup.5 or CONHSO.sub.2 R.sup.4 ;R.sup.4 and R.sup.5 independently represent hydrogen or C.sub.1 -C.sub.4 alkyl optionally substituted with one or more halogen atoms;R.sup.6 is a halogen atom or a group R.sup.4 ;R.sup.2 is hydrogen or halo; andR.sup.3 is C.sub.1 -C.sub.4 alkyl, C.sub.2 -C.sub.4 alkenyl or C.sub.2 -C.sub.4 alkynyl, any of which may optionally be substituted with one or more halogen atoms; or halo; or, where appropriate, a salt thereof;from a mixture containing the compound of general formula I together with one or more isomers or di-nitrated analogs thereof; the process comprising dissolving the mixture in a suitable crystallization solvent and recrystallizing the product from the resulting crystallization solution wherein the crystallization solution contains not more than 25% loading of the compound of general formula I, loading being defined as: ##EQU1## and wherein the temperature to which the solution is cooled for crystallization is not greater than about 30.degree. C.; wherein, after the addition of the crystallizing solvent but before recrystallization, the crystallization solution is subjected to at least one wash with an aqueous solution having an acid pH. The process is particularly useful for purifying acifluorfen produced via a route starting with m-cresol.

Abstract translation: 一种用于纯化通式I化合物的方法：其中R 1是氢或C 1 -C 6烷基，C 2 -C 6烯基或C 2 -C 6炔基，其中任何一个可任选被一个或多个选自卤素和羟基的取代基取代 ; 或COOR4，COR6，CONR4R5或CONHSO2R4; R4和R5独立地表示氢或任选被一个或多个卤素原子取代的C 1 -C 4烷基; R6是卤素原子或基团R4; R2是氢或卤素; 并且R 3是C 1 -C 4烷基，C 2 -C 4烯基或C 2 -C 4炔基，其中任何一个可任选地被一个或多个卤素原子取代; 或卤素; 或者在适当情况下为其盐; 由含有通式I化合物的混合物与一种或多种异构体或其二硝化类似物一起混合; 该方法包括将混合物溶解在合适的结晶溶剂中并从所得结晶溶液中重结晶产物，其中结晶溶液含有不超过25％的通式I化合物的负载，负载定义为：并且其中温度为 该溶液冷却结晶不超过约30℃。 其中，在加入结晶溶剂之后但重结晶之前，用酸性pH值的水溶液对结晶溶液进行至少一次洗涤。 该方法特别可用于纯化通过以间甲酚开始的途径产生的三氟果霜。

公开(公告)号：US5847240A

公开(公告)日：1998-12-08

申请号：US824654

申请日：1997-03-24

Applicant: Allen B. Quakenbush ,  Buford T. Pennington

Inventor： Allen B. Quakenbush ,  Buford T. Pennington

IPC: C06B21/00 ,  C06B25/04 ,  C07C201/16 ,  C07C205/00

CPC classification number: C06B21/0091 ,  C06B25/04 ,  C07C201/16

Abstract: A process is disclosed for removing a light organic compound from a liquid composition comprising said light organic compound in admixture with a nitroaromatic compound, said light organic compound having a partial vapor pressure in said composition that is greater than the partial vapor pressure of said nitroaromatic compound in said composition, said process comprising contacting said composition with steam or a gas to cause at least a portion of said light organic compound to pass out of said composition and into admixture with said steam or gas.

Abstract translation: 公开了一种从包含所述轻质有机化合物的液体组合物与硝基芳族化合物混合物中除去轻质有机化合物的方法，所述轻质有机化合物在所述组合物中的部分蒸汽压大于所述硝基芳族化合物的部分蒸汽压 在所述组合物中，所述方法包括使所述组合物与蒸汽或气体接触以使所述轻质有机化合物的至少一部分从所述组合物中排出并与所述蒸汽或气体混合。

公开(公告)号：US5710343A

公开(公告)日：1998-01-20

申请号：US809405

申请日：1997-05-08

Applicant: Reijo Johannes Backstrom

Inventor： Reijo Johannes Backstrom

IPC: C07C201/12 ,  C07C1/12 ,  C07C201/16 ,  C07C205/44 ,  C07C37/055

CPC classification number: C07C201/12 ,  C07C201/16

Abstract: The invention provides a method for the preparation of 3,4-dihydroxy-5-nitrobenzaldehyde by reacting 3-ethoxy-4-hydroxy-5-nitrobenzaldehyde with a reagent comprising zinc chloride, water and hydrogen chloride.

Abstract translation: PCT No.PCT / FI95 / 00513 Sec。 371日期：1997年5月8日 102（e）日期1997年5月8日PCT提交1995年9月20日PCT公布。 出版物WO96 / 09274 日期：1996年3月28日本发明提供通过使3-乙氧基-4-羟基-5-硝基苯甲醛与包含氯化锌，水和氯化氢的试剂反应来制备3,4-二羟基-5-硝基苯甲醛的方法。

公开(公告)号：US5567854A

公开(公告)日：1996-10-22

申请号：US532513

申请日：1995-09-22

Applicant: Wolfram Kissener ,  Herbert Emde ,  Achim Fessenbecker

Inventor： Wolfram Kissener ,  Herbert Emde ,  Achim Fessenbecker

IPC: C07C201/16 ,  C07C205/44 ,  C07C45/82

CPC classification number: C07C201/16

Abstract: 2- and 3-Nitrobenzaldehydes suitable for use as intermediates for the preparation of pharmaceuticals are obtained in a simple manner and without risk of uncontrolled decompositions by distilling mixtures of nitrobenzaldehyde isomers at bottom temperatures of at most 200.degree. C. in the presence of monomeric and/or polymeric aromatic amines and/or phenols and/or N- and S-containing phenothiazines.

Abstract translation: 适用于制备药物的中间体的2-和3-硝基苯甲醛以简单的方式获得，没有不受控制的分解的风险，通过在最多200℃的底部温度下蒸馏硝基苯甲醛异构体的混合物，在单体和/ /或聚合芳族胺和/或酚类和/或含N-和S-的吩噻嗪。

公开(公告)号：US5554299A

公开(公告)日：1996-09-10

申请号：US367873

申请日：1995-01-03

Applicant: Faouzi Joulak ,  Louis Le Bris ,  Philippe Marion

Inventor： Faouzi Joulak ,  Louis Le Bris ,  Philippe Marion

IPC: C02F1/66 ,  C02F9/00 ,  C07C201/16 ,  C02F1/52

CPC classification number: C02F1/66 ,  C07C201/16 ,  C02F2103/36 ,  Y10S210/909

Abstract: Objectionable byproduct aqueous effluents containing contaminating amounts of hydroxynitroaromatic compounds, in particular those aqueous effluents produced during the synthesis of nitroaromatic compounds, e.g., dinitrotoluenes, via reaction of an aromatic compound with nitric acid in the presence of sulfuric acid, are efficiently, facilely and economically treated/removed by (a) intimately contacting a mixture of at least one nitroaromatic compound and at least one hydroxynitroaromatic compound with an aqueous wash medium containing a neutralizing agent, (b) separating the resulting admixture into an organic phase and an aqueous phase, (c) recycling a fraction of the separated aqueous phase to the aqueous wash medium to thus constitute a portion thereof, and (d) periodically draining a fraction of the wash medium, whether to destruction thereof or to waste.

Abstract translation: 含有污染量的羟基硝基芳族化合物的有害副产物含水废水，特别是在硫酸存在下通过芳族化合物与硝酸的反应合成硝基芳族化合物（例如二硝基甲苯）期间产生的含水废水，是有效，便利和经济的 通过（a）使至少一种硝基芳族化合物和至少一种羟基硝基芳族化合物的混合物与含有中和剂的水性洗涤介质紧密接触来处理/除去，（b）将所得混合物分离成有机相和水相（ c）将分离的水相的一部分循环到水性洗涤介质中，从而构成其一部分，和（d）定期排出洗涤介质的一部分，不管其是否破坏或浪费。

公开(公告)号：US5500189A

公开(公告)日：1996-03-19

申请号：US383641

申请日：1995-02-06

Applicant: Minoru Morita ,  Keizo Takegami

Inventor： Minoru Morita ,  Keizo Takegami

IPC: C07B63/00 ,  B01D9/00 ,  B01D53/32 ,  B01D53/56 ,  B01D53/74 ,  B01J19/08 ,  C07C37/70 ,  C07C37/84 ,  C07C39/16 ,  C07C201/16 ,  C07C205/06 ,  C30B35/00

CPC classification number: B01J19/088 ,  B01D53/326 ,  B01D53/56 ,  B01D9/0004 ,  F23J2215/10 ,  F23J2219/201 ,  Y10T117/10

Abstract: Adiabatic self-evaporation cooling of a refrigerant is performed in a crystallizer for a treated organic matter which contains the refrigerant and is fed into the crystallizer. Crystals produced by the adiabatic self-evaporation cooling are withdrawn from the crystallize. An evaporated vapor is introduced from the crystallizer into an absorber so as to be contacted with a concentrated solution transformed from a generator for condensation in the absorber. A condensate is introduced from the absorber into the generator, the refrigerant is evaporated in the generator, an evaporated vapor is introduced from the generator to the condenser, the evaporated vapor is condensed in the condenser, a condensate is supplied from the condenser to the crystallizer and the concentrated solution is circulated between the absorber and the generator by returning the concentrated solution, in which the concentration of an absorbent is increased by the generator to the absorber.

Abstract translation: 制冷剂的绝热自蒸发冷却在用于含有制冷剂的处理过的有机物的结晶器中进行并进料到结晶器中。 由绝热自蒸发冷却产生的晶体从结晶中取出。 将蒸发的蒸气从结晶器引入吸收器，以便与从发生器转化的浓缩溶液接触以在吸收器中冷凝。 冷凝物从吸收器引入发生器，制冷剂在发生器中蒸发，蒸发的蒸汽从发生器引入冷凝器，蒸发的蒸气在冷凝器中冷凝，冷凝物从冷凝器供应到结晶器 并且浓缩溶液通过返回浓缩溶液在吸收器和发生器之间循环，其中吸收剂的浓度由发生器增加到吸收器。

公开(公告)号：US5446197A

公开(公告)日：1995-08-29

申请号：US78993

申请日：1993-06-17

Applicant: Mark Sandison ,  Ron Eva ,  Lawrence E. James

Inventor： Mark Sandison ,  Ron Eva ,  Lawrence E. James

IPC: C07C41/40 ,  C07C43/257 ,  C07C43/275 ,  C07C43/285 ,  C07C43/29 ,  C07C201/16 ,  C07C205/59 ,  C07C205/00

CPC classification number: C07C201/16

Abstract: A method of purifying acifluorfen to achieve a purity of greater than about 85% by weight involves heating to dissolution a solution of an acifluorfen crude wet cake and at least one solvent from the group of 1,2-dichlorobenzene, monochlorobenzene, o-xylene and p-xylene, with the solution having from about 10 to about 30 weight percent of acifluorfen crude wet cake. The-solution is then cooled until crystals of purified acifluorfen form. The crystals are then filtered at a temperature within the range of from about 0.degree. to about 30.degree. C. The filtered crystals are then recovered.

Abstract translation: 净化三氟果霜以达到大于约85重量％的纯度的方法涉及加热溶解氟锁草醚粗湿滤饼和至少一种来自1,2-二氯苯，一氯苯，邻二甲苯和 对二甲苯，溶液具有约10至约30重量％的三氟果霜粗湿饼。 然后将溶液冷却至纯化的三氟果霜形成晶体。 然后将晶体在约0℃至约30℃的温度范围内过滤。然后回收过滤的晶体。

公开(公告)号：US5409505A

公开(公告)日：1995-04-25

申请号：US876630

申请日：1992-04-30

Applicant: Minoru Morita ,  Keizo Takegami

Inventor： Minoru Morita ,  Keizo Takegami

IPC: C07B63/00 ,  B01D9/00 ,  B01D53/32 ,  B01D53/56 ,  B01D53/74 ,  B01J19/08 ,  C07C37/70 ,  C07C37/84 ,  C07C39/16 ,  C07C201/16 ,  C07C205/06 ,  B01D9/04 ,  C07C7/14 ,  C02F1/22

CPC classification number: B01J19/088 ,  B01D53/326 ,  B01D53/56 ,  B01D9/0004 ,  F23J2215/10 ,  F23J2219/201 ,  Y10T117/10

Abstract: Adiabatic self-evaporation cooling of a refrigerant is performed in a crystallizer for a treated organic matter which contains the refrigerant and is fed into the crystallizer. Crystals produced by the adiabatic self-evaporation cooling are withdrawn from the crystallize. An evaporated vapor is introduced from the crystallizer into an absorber so as to be contacted with a concentrated solution transformed from a generator for condensation in the absorber. A condensate is introduced from the absorber into the generator, the refrigerant is evaporated in the generator, an evaporated vapor is introduced from the generator to the condenser, the evaporated vapor is condensed in the condenser, a condensate is supplied from the condenser to the crystallizer and the concentrated solution is circulated between the absorber and the generator by returning the concentrated solution, in which the concentration of an absorbent is increased by the generator to the absorber.

Abstract translation: 制冷剂的绝热自蒸发冷却在用于含有制冷剂的处理过的有机物的结晶器中进行并进料到结晶器中。 由绝热自蒸发冷却产生的晶体从结晶中取出。 将蒸发的蒸气从结晶器引入吸收器，以便与从发生器转化的浓缩溶液接触以在吸收器中冷凝。 冷凝物从吸收器引入发生器，制冷剂在发生器中蒸发，蒸发的蒸气从发生器引入冷凝器，蒸发的蒸气在冷凝器中冷凝，冷凝物从冷凝器供应到结晶器 并且浓缩溶液通过返回浓缩溶液在吸收器和发生器之间循环，其中吸收剂的浓度由发生器增加到吸收器。

公开(公告)号：US5180859A

公开(公告)日：1993-01-19

申请号：US910005

申请日：1992-07-07

Applicant: Larry D. Timberlake ,  James L. Brennan

Inventor： Larry D. Timberlake ,  James L. Brennan

IPC: C07C201/12 ,  C07C201/16 ,  C07C205/08

CPC classification number: C07C201/16 ,  C07C201/12

Abstract: A process for the preparation of halonitroalkanes, e.g. bromonitromethane, is disclosed in which a nitroalkane is reacted with an alkali metal base or an alkaline earth metal base, and the resulting nitroalkane salt is halogenated to form the halonitroalkane in a reaction mixture. The process is improved by acidifying the reaction mixture, preferably to pH=0-4, and thereafter recovering the halonitroalkane by azeotropic distillation of the reaction mixture. The acidification step increases the amount of halonitroalkane recovered, as compared to prior art processes in which the reaction mixture is distilled without prior acidification.

Abstract translation: 一种制备卤代硝基烷烃的方法，例如 溴硝基甲烷，其中硝基烷烃与碱金属碱或碱土金属碱反应，并将所得的硝基烷烃卤化以在反应混合物中形成卤代硝基烷烃。 通过酸化反应混合物，优选至pH = 0-4，然后通过反应混合物的共沸蒸馏回收卤代硝基烷烃来改进该方法。 与现有技术的方法相比，酸化步骤增加了所回收的卤代硝基烷烃的量，其中在没有预先酸化的情况下蒸馏反应混合物。

公开(公告)号：US5149890A

公开(公告)日：1992-09-22

申请号：US786479

申请日：1991-11-01

Applicant: Gunther Rauchschwalbe ,  Heinz-Ulrich Blank ,  Ludwig Deibele ,  Kaspar Hallenberger ,  Gerhard Ruffert

Inventor： Gunther Rauchschwalbe ,  Heinz-Ulrich Blank ,  Ludwig Deibele ,  Kaspar Hallenberger ,  Gerhard Ruffert

IPC: C07C201/16 ,  C07C205/06

CPC classification number: C07C201/16

Abstract: Pure or substantially enriched 2,4- and 2,6-dinitrotoluene can be isolated from a mixture containing these isomers if such a mixture is distilled under a pressure of 0.5 to 20 mbar at a temperature of 80.degree. to 200.degree. C. with exclusion of reducing conditions.

Abstract translation: 如果将这种混合物在0.5至20毫巴的压力下在80至200℃的温度下蒸馏而排除，则纯的或基本上富含的2,4-和2,6-二硝基甲苯可以从含有这些异构体的混合物中分离出来 的减少条件。