公开(公告)号：US4429169A

公开(公告)日：1984-01-31

申请号：US372055

申请日：1982-04-26

Applicant: Gerd Leston

Inventor： Gerd Leston

IPC: C07C37/86 ,  C07C201/16 ,  C07C205/22 ,  C07C37/68

CPC classification number: C07C37/86 ,  C07C37/685 ,  C07C37/84

Abstract: A process is disclosed for separating 5-isopropyl-m-cresol from other isopropylated m-cresols by treating a mixture of the isopropylated m-cresols with a metal halide salt. The metal halide salt preferentially forms a complex with 5-isopropyl-m-cresol over other related closely-boiling isopropylated m-cresols in the mixture. The preferentially-formed complex of 5-isopropyl-m-cresol may then be isolated from the mixture and the complex decomposed to provide a product substantially enriched in, or substantially entirely composed of, 5-isopropyl-m-cresol. The process is particularly suitable for isolating 5-isopropyl-m-cresol from closely-boiling isomers, and diisopropylated m-cresols.

Abstract translation: 公开了通过将异丙基化间甲酚与金属卤化物盐的混合物进行处理从其它异丙基化间甲酚中分离5-异丙基间甲酚的方法。 与其他相关的沸点相近的异丙基化间甲酚相比，金属卤化物盐与5-异丙基间甲酚优先形成络合物。 然后可以从混合物中分离出优先形成的5-异丙基间甲酚的复合物，并将络合物分解，得到基本上富含或完全由5-异丙基间甲酚组成的产物。 该方法特别适用于从紧密沸腾的异构体中分离出5-异丙基间甲酚和二异丙基间甲酚。

公开(公告)号：US3992455A

公开(公告)日：1976-11-16

申请号：US402160

申请日：1973-10-01

Applicant: Gerd Leston

Inventor： Gerd Leston

IPC: C07C27/00 ,  C07C37/00 ,  C07C37/14 ,  C07C37/74 ,  C07C39/06 ,  C07C39/15 ,  C07C39/16 ,  C07C67/00

CPC classification number: C07C37/14 ,  C07C37/00 ,  C07C37/74 ,  C07C39/06 ,  C07C39/15 ,  C07C2101/14

Abstract: This disclosure is directed to a method for preparing 5-sec-alkyl-m-cresol in high concentrations and yields comprising alkylating m-cresol with an alkene over a solid catalyst selected from finely divided silica alumina clays and finely divided molecular sieves and then isomerizing the alkylated m-cresol product over the same catalyst for at least two hours at temperatures of at least about 250.degree. C. The ratio of alkene to m-cresol is from about 0.5:1.0 to about 1.0:1.0. The resulting isomerized alkylated m-cresol contains a ratio of 5-alkyl-m-cresol to 6-alkyl-m-cresol of at least 2.5:1 and a ratio of 5-alkyl-m-cresol to 4-alkyl-m-cresol of at least 3.0:1.0. The desired 5-alkyl-m-cresol may be obtained from the isomerized alkylated-m-cresol reaction product by fractional distillation. The undesired alkylated-m-cresol isomers and unreacted m-cresol may be recycled into the alkylation and/or isomerization step. The method is particularly useful for preparing 5-isopropyl-m-cresol(m-thymol).

Abstract translation: 本公开涉及一种高浓度制备5-仲烷基间甲酚的方法，其产率包括在间歇甲酚与烯烃的烷基化作用下，在选自细碎二氧化硅氧化铝粘土和细碎分子筛的固体催化剂上进行异构化 在相同催化剂上的烷基化间甲酚产物在至少约250℃的温度下至少两小时。烯烃与间甲酚的比例为约0.5:1.0至约1.0:1.0。 所得异构化烷基化间甲酚的5-烷基间甲酚与6-烷基间甲酚的比例至少为2.5:1，5-烷基间甲酚与4-烷基 - 间甲酚的比例为 甲酚至少3.0：1.0。 所需的5-烷基间甲酚可以通过分馏由异构化的烷基化间甲酚反应产物获得。 不需要的烷基化间甲酚异构体和未反应的间甲酚可以再循环到烷基化和/或异构化步骤中。 该方法特别适用于制备5-异丙基间甲酚（间百里酚）。

公开(公告)号：US4496774A

公开(公告)日：1985-01-29

申请号：US633717

申请日：1984-07-23

Applicant: Gerd Leston

Inventor： Gerd Leston

IPC: C07C37/86 ,  C07C39/06 ,  C07C201/16 ,  C07C205/22

CPC classification number: C07C201/16 ,  C07C37/86 ,  C07C39/06

Abstract: A process is disclosed for separating nitrated phenolic compounds from other nitrated and unnitrated phenolics by treating a mixture of the phenolics with a metal halide salt. The metal halide salt preferentially forms a complex with one of the phenolics over other related phenolics in the mixture. The preferentially-formed complex of one of the phenolics may then be isolated from the mixture and the complex decomposed to provide a product substantially enriched in, or substantially entirely composed of, one phenolic. The process is particularly suitable for resolving a mixture comprising phenol or cresol from their ortho-nitrated derivatives, or a mixture of two isomeric nitrated phenols or cresols or a mixture of mono- and dinitrated phenols or cresols.

Abstract translation: 公开了通过将酚类与金属卤化物盐的混合物进行处理来分离硝化酚类化合物与其它硝化和未硝化酚醛树脂的方法。 与混合物中的其它相关酚类物质相比，金属卤化物盐优先与酚类之一形成络合物。 然后可以从混合物中分离一种酚类的优先形成的络合物，并且复合物被分解以提供基本上富含或完全由一种酚类组成的产物。 该方法特别适用于从其邻硝化衍生物或两种异构硝化酚或甲酚的混合物或单硝化苯酚或二硝基苯酚或甲酚的混合物中分离出包含苯酚或甲酚的混合物。

公开(公告)号：US4475001A

公开(公告)日：1984-10-02

申请号：US476060

申请日：1983-03-17

Applicant: Gerd Leston

Inventor： Gerd Leston

IPC: C07C37/00 ,  C07C37/50 ,  C07C39/06

CPC classification number: C07C37/50

Abstract: Ortho- or para-monoalkylated phenols or 2,4- or 2,6-dialkylphenols can be produced from phenolic compounds in good yields and in the absence of isomers. The starting phenol which has at least two available ortho or para positions unsubstituted is converted to a t-alkylated phenol having at least one ortho or para position unsubstituted. The desired t-alkylated phenolic compound is reacted with an aldehyde having one to four carbon atoms and a secondary aliphatic or alicyclic amine. The reaction is conducted in the liquid phase with a stoichiometric amount of the phenolic compound and stoichiometric or excess of stoichiometric amounts of the aldehyde and the secondary amine. The reaction is conducted at a temperature in the range of about 0.degree. C., to about 100.degree. C. and the reaction produces an aminoalkylated t-alkylated phenol. The aminoalkylated phenol is contacted with hydrogen in the presence of a metal catalyst at a temperature of about 100.degree. C. to about 175.degree. C. at a hydrogen pressure not greater than 500 psi to produce monoalkylated, mono- or di-t-alkylated phenol or a dialkylated, mono-t-alkylated phenol in the ortho- and para- positions. The thus produced alkylated t-alkylated phenolic compound is contacted with an acid or an acid reacting substance to give the desired alkylated phenolic compound. These compounds are separated to produce ortho-monoalkylated, para-monoalkylphenol, 2,4-dialkylphenol and 2,6-dialkylphenol.

Abstract translation: 正烷基或对位单烷基化酚或2,4-或2,6-二烷基酚可以以良好的产率和不存在异构体由酚类化合物制备。 具有至少两个可用的未取代的邻位或对位的起始苯酚转化为具有至少一个未取代的邻位或对位的叔烷基化苯酚。 所需的叔烷基化酚类化合物与具有1-4个碳原子的醛和仲脂族或脂环族胺反应。 反应在液相中以化学计量的酚类化合物和化学计量或过量的化学计量量的醛和仲胺进行。 反应在约0℃至约100℃的温度下进行，反应产生氨基烷基化的t-烷基化苯酚。 氨基烷基化苯酚在金属催化剂存在下，在氢气压力不大于500psi的温度下，在大约100℃至大约175℃的温度下与氢气接触，以产生单烷基化，单烷基化或二烷基化 苯酚或邻位和对位的二烷基化单叔烷基化苯酚。 由此制得的烷基化的叔烷基化的酚类化合物与酸或酸反应物质接触，得到所需的烷基化酚类化合物。 这些化合物被分离以产生邻 - 单烷基化的对 - 单烷基苯酚，2,4-二烷基苯酚和2,6-二烷基苯酚。

公开(公告)号：US4447654A

公开(公告)日：1984-05-08

申请号：US431640

申请日：1982-09-30

Applicant: Gerd Leston

Inventor： Gerd Leston

IPC: C07C201/16 ,  C07C79/22

CPC classification number: C07C201/16

Abstract: A process is disclosed for separating nitrated phenolic compounds from other nitrated and unnitrated phenolics by treating a mixture of the phenolics with a metal halide salt. The metal halide salt preferentially forms a complex with one of the phenolics over other related phenolics in the mixture. The preferentially-formed complex of one of the phenolics may then be isolated from the mixture and the complex decomposed to provide a product substantially enriched in, or substantially entirely composed of, one phenolic. The process is particularly suitable for resolving a mixture comprising phenol or cresol from their ortho-nitrated derivatives, or a mixture of two isomeric nitrated phenols or cresols or a mixture of mono-and dinitrated phenols or cresols.

Abstract translation: 公开了通过将酚类与金属卤化物盐的混合物进行处理来分离硝化酚类化合物与其它硝化和未硝化酚醛树脂的方法。 与混合物中的其它相关酚类物质相比，金属卤化物盐优先与酚类之一形成络合物。 然后可以从混合物中分离一种酚类的优先形成的络合物，并且复合物被分解以提供基本上富含或完全由一种酚类组成的产物。 该方法特别适用于从其邻硝化衍生物或两种异构硝化酚或甲酚的混合物或单硝酸盐和二硝基苯酚或甲酚的混合物中分离出包含苯酚或甲酚的混合物。

公开(公告)号：US4267390A

公开(公告)日：1981-05-12

申请号：US53195

申请日：1979-06-29

Applicant: Gerd Leston

Inventor： Gerd Leston

IPC: C07C37/86 ,  C07C37/68 ,  C07C37/74

CPC classification number: C07C37/86 ,  C07C37/685 ,  C07C37/84

Abstract: A process is disclosed for the stepwise separation of para-cresol and meta-cresol from a mixture of methylated and ethylated phenols. The para-cresol forms a complex with a dehydrated or anhydrous inorganic halide salt selected from the group consisting of calcium bromide, lithium bromide, manganese bromide and magnesium chloride. The meta-cresol isomer is separated from the mixture by formation of a complex with sodium acetate. Where the anhydrous or dehydrated inorganic halide salt is added firstly to the mixture of methylated and ethylated phenols including para-cresol and meta-cresol, the halide salt is provided in an amount to give a mole ratio of the halide salt to para-cresol in the mixture in the range of about 0.5 to one to about 1.5 to one. The para-cresol complexes with the halide salt and the complex is then removed from the mixture. The para-cresol-salt complex is thereafter decomposed to recover the para-cresol. The mixture of methylated and ethylated phenols including meta-cresol from which the para-cresol has been removed has added to it sodium acetate in an amount to give a mole ratio of sodium acetate to meta-cresol in the mixture in the range of about 0.5 to one to about 5 to one. The meta-cresol sodium acetate complex is then separated from the mixture of methylated and ethylated phenols and thereafter the complex is decomposed to produce a high purity meta-cresol. It is a feature of the invention that either of the complexing steps may be performed first; that is, either of the anhydrous halide salt or the sodium acetate may be added to the mixture, followed thereafter by addition of the other complexing agent.

Abstract translation: 公开了从甲基化和乙基化酚的混合物中逐步分离对甲酚和间甲酚的方法。 对甲酚与选自溴化钙，溴化锂，溴化锰和氯化镁的脱水或无水无机卤化物盐形成络合物。 通过与乙酸钠形成络合物将间甲酚异构体与混合物分离。 当将无水或脱水的无机卤化物盐首先加入到甲基化和乙基化酚（包括对甲酚和间甲酚）的混合物中时，卤化物盐的用量使卤化物盐与对甲酚的摩尔比在 该混合物的范围为约0.5至1至约1.5比1。 然后从混合物中除去与卤化物盐和络合物的对甲酚配合物。 然后将对甲酚盐复合物分解，以回收对甲酚。 已经除去对甲酚的甲基化和乙基化酚包括间甲酚的混合物已经向其中加入了乙酸钠，其量使混合物中乙酸钠与间甲酚的摩尔比在约0.5的范围内 到1到5到1。 然后从甲基化和乙基化酚的混合物中分离出间甲酚醋酸钠络合物，然后分解该复合物以产生高纯度的间甲酚。 本发明的特征在于可以首先执行任一个复合步骤; 也就是说，可以向混合物中加入无水卤化物盐或乙酸钠，然后加入另外的络合剂。

公开(公告)号：US4499312A

公开(公告)日：1985-02-12

申请号：US582082

申请日：1984-02-21

Applicant: Gerd Leston

Inventor： Gerd Leston

IPC: C07C37/86 ,  C07C39/06

CPC classification number: C07C37/86 ,  C07C37/84 ,  C07C39/235

Abstract: A process is disclosed for separating 3,5-xylenol or 3,4-xylenol from other closely boiling polymethylated phenolics by treating a mixture of the phenolics with a metal halide salt. The metal halide salt preferentially forms a complex with the xylenol over other related phenolics in the mixture. The preferentially-formed complex of the xylenol may then be isolated from the mixture and the complex decomposed to provide a product substantially enriched in, or substantially entirely composed of the xylenol.

Abstract translation: 公开了通过将酚类与金属卤化物盐的混合物进行处理从其它紧密沸腾的多甲基化酚类中分离3,5-二甲苯酚或3,4-二甲苯酚的方法。 金属卤化物盐与混合物中的其它相关酚类优先与二甲苯酚形成络合物。 然后可以从混合物中分离优先形成的二甲苯酚复合物，并且复合物分解以提供基本上富含或完全由二甲苯酚组成的产物。

公开(公告)号：US4479019A

公开(公告)日：1984-10-23

申请号：US582083

申请日：1984-02-21

Applicant: Gerd Leston

Inventor： Gerd Leston

IPC: C07C201/16 ,  C07C205/22 ,  C07C79/32

CPC classification number: C07C201/16 ,  C07C205/22

Abstract: A process is disclosed for separating nitrated phenolic compounds from other nitrated and unnitrated phenolics by treating a mixture of the phenolics with a metal halide salt. The metal halide salt preferentially forms a complex with one of the phenolics over other related phenolics in the mixture. The preferentially-formed complex of one of the phenolics may then be isolated from the mixture and the complex decomposed to provide a product substantially enriched in, or substantially entirely composed of, one phenolic. The process is particularly suitable for resolving a mixture comprising phenol or cresol from their ortho-nitrated derivatives, or a mixture of two isomeric nitrated phenols or cresols or a mixture of mono-and dinitrated phenols or cresols.

Abstract translation: 公开了通过将酚类与金属卤化物盐的混合物进行处理来分离硝化酚类化合物与其它硝化和未硝化酚醛树脂的方法。 与混合物中的其它相关酚类物质相比，金属卤化物盐优先与酚类之一形成络合物。 然后可以从混合物中分离一种酚类的优先形成的络合物，并且复合物被分解以提供基本上富含或完全由一种酚类组成的产物。 该方法特别适用于从其邻硝化衍生物或两种异构硝化酚或甲酚的混合物或单硝酸盐和二硝基苯酚或甲酚的混合物中分离出包含苯酚或甲酚的混合物。

公开(公告)号：US4447658A

公开(公告)日：1984-05-08

申请号：US431651

申请日：1982-09-30

Applicant: Gerd Leston

Inventor： Gerd Leston

IPC: C07C37/86 ,  C07C37/68

CPC classification number: C07C37/86 ,  C07C37/685 ,  C07C37/84

Abstract: A process is disclosed for separating 3,5-xylenol or 3,4-xylenol from other closely boiling polymethylated phenolics by treating a mixture of the phenolics with a metal halide salt. The metal halide salt preferentially forms a complex with the xylenol over other related phenolics in the mixture. The preferentially-formed complex of the xylenol may then be isolated from the mixture and the complex decomposed to provide a product substantially enriched in, or substantially entirely composed of the xylenol.

Abstract translation: 公开了通过将酚类与金属卤化物盐的混合物进行处理从其它紧密沸腾的多甲基化酚类中分离3,5-二甲苯酚或3,4-二甲苯酚的方法。 金属卤化物盐与混合物中的其它相关酚类优先与二甲苯酚形成络合物。 然后可以从混合物中分离优先形成的二甲苯酚复合物，并且复合物分解以提供基本上富含或完全由二甲苯酚组成的产物。

公开(公告)号：US4424381A

公开(公告)日：1984-01-03

申请号：US372062

申请日：1982-04-26

Applicant: Gerd Leston

Inventor： Gerd Leston

IPC: C07C37/86 ,  C07C37/68

CPC classification number: C07C37/86 ,  C07C37/685 ,  C07C37/84

Abstract: A process is disclosed for separating closely-boiling dihydric phenol compounds by treating a mixture of dihydric phenols with a metal halide salt. The metal halide salt preferentially forms a complex with one of the dihydric phenols over other related dihydric phenols in the mixture. The preferentially-formed complex of one of the dihydric phenols may then be isolated from the mixture and the complex decomposed to provide a product substantially enriched in, or substantially entirely composed of, one dihydric phenol. The process is particularly suitable for resolving a mixture comprising hydroquinone and catechol, or a mixture of hydroquinone and resorcinol, or a mixture of homocatechol and hydroquinone, or a mixture of catechol and resorcinol.

Abstract translation: 公开了通过处理二元酚与金属卤化物盐的混合物来分离紧密沸腾的二元酚化合物的方法。 金属卤化物盐与混合物中的其它相关二元酚优先与二元酚之一形成络合物。 然后可以从混合物中分离一种二元酚的优先形成的络合物，并且络合物被分解以提供基本上富含或完全由一元二酚构成的产物。 该方法特别适用于分离包含对苯二酚和儿茶酚，或氢醌和间苯二酚的混合物，或高聚邻苯二酚和氢醌混合物，或邻苯二酚和间苯二酚的混合物的混合物。