公开(公告)号：US20090177012A1

公开(公告)日：2009-07-09

申请号：US11718526

申请日：2005-10-20

申请人： Tsuyoshi Fukuhara ,  Shoji Hara ,  Toshio Hidaka

发明人： Tsuyoshi Fukuhara ,  Shoji Hara ,  Toshio Hidaka

IPC分类号： C07C209/00

CPC分类号： C07C209/74 ,  C07C213/08 ,  C07D233/02 ,  C07C211/29 ,  C07C217/58

摘要： A process for producing an α,α-difluoroamine which comprises using hydrogen fluoride and a Lewis base in specific amounts in the halogen-fluorine exchange reaction using an α,α-dihaloamine as the substrate. The process can be industrially applied, enables to obtain the object compound in a short time at a great yield and can be conducted easily with excellent productivity.

摘要翻译： 一种制备α，α-二氟胺的方法，其包括使用α，α-二卤代胺作为底物，在卤素 - 氟交换反应中使用氟化氢和具有特定量的路易斯碱。 该工艺可以在工业上应用，能够在短时间内以大的收率获得目标化合物，并且可以以优异的生产率容易地进行。

公开(公告)号：US20060167324A1

公开(公告)日：2006-07-27

申请号：US10512990

申请日：2003-04-24

申请人： Toshio Hidaka ,  Norio Fushimi ,  Takafumi Yoshimura ,  Takeshi Kawai

发明人： Toshio Hidaka ,  Norio Fushimi ,  Takafumi Yoshimura ,  Takeshi Kawai

IPC分类号： C07C25/13

CPC分类号： C07C45/41 ,  C07B39/00 ,  C07C29/147 ,  C07C39/24 ,  C07C45/45 ,  C07C45/63 ,  C07C47/55 ,  C07C49/80 ,  C07C51/04 ,  C07C51/62 ,  C07C67/307 ,  C07C211/29 ,  C07C233/65 ,  C07C255/50 ,  C07C63/72 ,  C07C63/70 ,  C07C69/76 ,  C07C33/46

摘要： The process for producing a (fluoroalkyl)benzene derivative according to the present invention comprises a step of reducing the total content of group 3 to group 12 transition metals in an alkylbenzene derivative to 500 ppm or less in terms of metal atoms; a step of halogenating the branched alkyl group of the purified alkylbenzene derivative by a photohalogenation to obtain a (haloalkyl)benzene derivative; and a step of subjecting the (haloalkyl)benzene derivative to a halogen-fluorine exchange using HF in an amount of 10 mol or higher per one mole of the (haloalkyl)benzene derivative. The (fluoroalkyl)benzene derivative produced by the process is reduced in the content of impurities such as residual halogens and residual metals, and is useful as intermediates for functional chemical products for use in applications such as medicines and electronic materials.

摘要翻译： 本发明的（氟代烷基）苯衍生物的制造方法包括使烷基苯衍生物中的第1族第1族过渡金属的含量以金属原子换算为500ppm以下的步骤; 通过光卤化来卤化纯化的烷基苯衍生物的支链烷基以获得（卤代烷基）苯衍生物的步骤; 以及使用每10摩尔（卤代烷基）苯衍生物为10摩尔以上的HF的（卤代烷基）苯衍生物进行卤 - 氟交换的工序。 通过该方法制备的（氟代烷基）苯衍生物的残留卤素和残余金属等杂质含量降低，可用作药物和电子材料等应用中的功能性化学产品的中间体。

公开(公告)号：US20060161028A1

公开(公告)日：2006-07-20

申请号：US10545005

申请日：2004-02-10

申请人： Toshio Hidaka ,  Takafumi Yoshimura ,  Yoshifumi Sato ,  Norio Fushimi ,  Masaharu Doya

发明人： Toshio Hidaka ,  Takafumi Yoshimura ,  Yoshifumi Sato ,  Norio Fushimi ,  Masaharu Doya

IPC分类号： C07C17/00

CPC分类号： C07C253/30 ,  C07B39/00 ,  C07C17/12 ,  C07C17/156 ,  C07C17/158 ,  C07C51/363 ,  C07C51/43 ,  C07C25/02 ,  C07C25/13 ,  C07C25/18 ,  C07C25/125 ,  C07C63/70 ,  C07C255/50

摘要： Provided is a production method for an iodine compound in which iodine is reacted with a substrate in the presence of a porous material having a pore diameter of 500 nm or less or in the presence of the above porous material and an oxidizing agent and a production process for high purity 5-iodo-2-methylbenzoic acid comprising an iodination reaction step carried out by the above-mentioned, a crystal precipitation and separation step in which a product is precipitated by adding water or cooling and then separated and a purification step in which crystal separated is recrystallized using an organic solvent. According to the production method for an iodine compound described above, iodine can be introduced into various substrates at a high selectivity. Since expensive metals and specific reagents do not have to be used, it can readily be carried out in an industrially scale, and the product having a high purity can be obtained. Further, the process comprising the iodination reaction, separation and purification steps described above makes it possible to readily obtain at a high yield, 5-iodo-2-methylbenzoic acid having a high purity which is useful in uses for functional chemical products such as medicines. The process of the present invention comprising iodination reaction, separation and purification steps is characterized by that it is simple in terms of a procedure and that the purification load is smaller, and it is very advantageous in industrially carrying out.

摘要翻译： 提供一种碘化合物的制造方法，其中碘在孔径为500nm以下的多孔质材料的存在下，或者在上述多孔质材料和氧化剂的存在下，与基材反应，制造方法 包括通过上述进行的碘化反应步骤的高纯度5-碘-2-甲基苯甲酸，其中通过加入水或冷却然后分离产物而沉淀产物的晶体沉淀和分离步骤和纯化步骤，其中 使用有机溶剂重结晶晶体分离。 根据上述碘化合物的制造方法，能够以高选择性将碘引入各种基材中。 由于不需要使用昂贵的金属和特定试剂，因此可以容易地以工业规模进行，可以获得高纯度的产物。 此外，包括上述碘化反应，分离和纯化步骤的方法使得可以容易地以高产率获得具有高纯度的5-碘-2-甲基苯甲酸，其可用于诸如药物的功能性化学产品的用途 。 包括碘化反应，分离和纯化步骤的本发明方法的特征在于它在程序方面简单，净化负荷较小，在工业上非常有利。

公开(公告)号：US20060141591A1

公开(公告)日：2006-06-29

申请号：US10559577

申请日：2004-05-31

申请人： Youichi Kyuuko ,  Sachiko Koshiishi ,  Toshio Hidaka

发明人： Youichi Kyuuko ,  Sachiko Koshiishi ,  Toshio Hidaka

IPC分类号： C12P17/06 ,  C07D311/04

CPC分类号： C12P17/06 ,  C12P41/004

摘要： In the method for producing an optically active chromancarboxylate of the present invention, one of the enantiomers of racemic chromancarboxylic acid is esterified in a solvent containing an alcohol in the presence of a biocatalyst. After the esterification, the other enantiomer, i.e., the non-reacted chromancarboxylic acid is separated out of the reaction mixture to obtain the aimed optically active ester. The optically active chromancarboxylate is useful as the material for medicines, agricultural chemicals, etc. The invention provides an efficient production method thereof which is industrially applicable.

摘要翻译： 在本发明的光学活性色淀羧酸盐的制造方法中，在生物催化剂存在下，将含有醇的溶剂中的外消旋二羧酸的对映异构体酯化。 酯化后，从反应混合物中分离出另一种对映异构体，即未反应的色原羧酸，得到目标光学活性酯。 光学活性色淀羧酸盐可用作药物，农药等的材料。本发明提供了其在工业上可应用的有效的制备方法。

公开(公告)号：US08093429B2

公开(公告)日：2012-01-10

申请号：US12302362

申请日：2007-05-31

申请人： Toshio Hidaka ,  Takafumi Yoshimura ,  Shoji Hara ,  Tsuyoshi Fukuhara

发明人： Toshio Hidaka ,  Takafumi Yoshimura ,  Shoji Hara ,  Tsuyoshi Fukuhara

IPC分类号： C07C211/27

CPC分类号： C07C211/29 ,  C07C231/12 ,  Y02P20/582 ,  C07C233/65

摘要： Provided are a fluorous-tag-introduced fluoroamine of a general formula (I), its production method, a method of fluorination of a substrate having functional group containing oxygen with the fluoroamine serving as a fluorinating agent, and a method of recovering a fluorous-tag-introduced amide after the fluorination. The fluoroamine and its production method, as well as the fluorination method with the fluoroamine and the method of recovery of a fluorous-tag-introduced amide are ecological and advantageous in industrial use, as the load for separating and collecting the product after the fluorination with the fluoroamine serving as a fluorinating agent is small. (In the formula, R0 is an alkyl group or an aryl group having substituent(s) of Rf—(CH2)m—; Rf is a perfluoroalkyl group; m is from 0 to 2; R1 and R2 each are an alkyl group or an aryl group.)

摘要翻译： 提供了通式（I）的氟标记导入的氟胺，其制备方法，含氟氧基官能团的底物氟化作为氟化剂的方法，以及回收氟 - 标签引入酰胺后氟化。 氟胺及其制备方法以及氟胺的氟化方法和引入氟标签的酰胺的回收方法在工业上是生态和有利的，作为在氟化后分离和收集产物的负载 作为氟化剂的氟胺是小的。 （式中，R 0为具有Rf - （CH 2）m - 的取代基的烷基或芳基，Rf为全氟烷基，m为0〜2，R 1和R 2各自为烷基或 芳基）

公开(公告)号：US08080676B2

公开(公告)日：2011-12-20

申请号：US12312125

申请日：2007-10-25

申请人： Akifumi Iida ,  Youichi Kyuuko ,  Toshio Hidaka

发明人： Akifumi Iida ,  Youichi Kyuuko ,  Toshio Hidaka

IPC分类号： C07D311/66

CPC分类号： C07D311/66 ,  C07B53/00

摘要： The present invention provides an industrially available method for efficiently producing high-purity S-(−)-6-hydroxy-2,5,7,8-tetramethylchromane-2-carboxylic acid excellent in solid-liquid separability from an S-(−)-6-hydroxy-2,5,7,8-tetramethylchromane-2-carboxylic acid ester, and also provides products obtained by the method.Under a temperature condition of 50-80° C. in an aqueous solvent, (A) an S-(−)-6-hydroxy-2,5,7,8-tetramethylchromane-2-carboxylic acid ester represented by the general formula (1) is hydrolyzed under a basic condition for 1-3 hours; then (B) the insoluble matters contained in the reaction solution resulting from the hydrolysis are removed; and (C) an acid is added to the resulting solution to effect crystallization; provided that R in the general formula (1) represents an alkyl or aryl group.

摘要翻译： 本发明提供了一种工业上可行的方法，用于有效地生产出S-（ - ） - （ - ） - 羟基-2,5,7,8-四甲基苯并二氢吡喃-2-羧酸的固 - 液分离性优异的高纯度S - （ - ） - ）-6-羟基-2,5,7,8-四氢苯并二氢吡喃-2-羧酸酯，并且还提供通过该方法获得的产物。 在水性溶剂中在50-80℃的温度条件下，（A）由通式（A）表示的S - （ - ） - 6-羟基-2,5,7,8-四氢苯并二氢吡喃-2-羧酸酯 （1）在碱性条件下水解1-3小时; 然后（B）去除由水解产生的反应溶液中所含的不溶物; 和（C）向所得溶液中加入酸以进行结晶; 条件是通式（1）中的R表示烷基或芳基。

公开(公告)号：US07829741B2

公开(公告)日：2010-11-09

申请号：US11718526

申请日：2005-10-20

申请人： Tsuyoshi Fukuhara ,  Shoji Hara ,  Toshio Hidaka

发明人： Tsuyoshi Fukuhara ,  Shoji Hara ,  Toshio Hidaka

IPC分类号： C07C209/68 ,  C07C209/74

CPC分类号： C07C209/74 ,  C07C213/08 ,  C07D233/02 ,  C07C211/29 ,  C07C217/58

摘要： A process for producing an α,α-difluoroamine which comprises using hydrogen fluoride and a Lewis base in specific amounts in the halogen-fluorine exchange reaction using an α,α-dihaloamine as the substrate. The process can be industrially applied, enables to obtain the object compound in a short time at a great yield and can be conducted easily with excellent productivity.

摘要翻译： 一种制备α，α-二氟胺的方法，其包括使用α，α-二卤代胺作为底物，在卤素 - 氟交换反应中使用氟化氢和路易斯碱。 该工艺可以在工业上应用，能够在短时间内以大的收率获得目标化合物，并且可以以优异的生产率容易地进行。

公开(公告)号：US07297821B2

公开(公告)日：2007-11-20

申请号：US11297408

申请日：2005-12-09

申请人： Toshio Hidaka ,  Norio Fushimi ,  Takafumi Yoshimura ,  Takeshi Kawai

发明人： Toshio Hidaka ,  Norio Fushimi ,  Takafumi Yoshimura ,  Takeshi Kawai

IPC分类号： C07C211/00

CPC分类号： C07F9/54 ,  C07B39/00 ,  C07C17/16 ,  C07C17/18 ,  C07C211/29 ,  C07C251/30 ,  C07C271/20 ,  C07F9/5004 ,  Y02P20/582

摘要： A fluorine compound represented by Formula (1) is provided. The above fluorine compound is effective for introducing a fluorine atom into a compound having an active group such as an oxygen-containing functional group, and it can be used for uses of surface treatment, cleaning and coating. Further, after the fluorination reaction, the above compound is recovered and can be reused as a starting material for producing the above fluorine compound, and it is useful for various fluorination processes. (wherein X represents a nitrogen or phosphorus atom; R0, R1, and R2 represent hydrogen, an alkyl group or aryl group which may have a substituent, and they each may be the same or different; and R0, R1, and R2 may be combined with each other to form a ring).

摘要翻译： 提供由式（1）表示的氟化合物。 上述氟化合物有效地将氟原子引入具有活性基团的化合物如含氧官能团，并且其可用于表面处理，清洁和涂覆的用途。 此外，在氟化反应之后，回收上述化合物，可以重复使用作为制备上述氟化合物的原料，可用于各种氟化处理。 （其中X表示氮或磷原子; R 0，R 1，R 2和R 2表示氢，烷基或芳基， 可以具有取代基，并且它们各自可以相同或不同;并且R 0，R 1和R 2可以与 彼此形成一个戒指）。

公开(公告)号：US20070179304A1

公开(公告)日：2007-08-02

申请号：US10587545

申请日：2005-01-28

申请人： Kazuo Tanaka ,  Youichi Kyuuko ,  Toshio Hidaka

发明人： Kazuo Tanaka ,  Youichi Kyuuko ,  Toshio Hidaka

IPC分类号： C07D311/04

CPC分类号： C07D311/66 ,  C07D311/62

摘要： The invention provides a process for producing a chroman compound represented by formula (1), characterized in that the process includes allowing a phenol, an unsaturated compound, and a formaldehyde to react in the absence of catalyst and in the presence of water in an amount by mole 1 to 10 times that of the phenol. According to the present invention, a high-purity chroman compound can be produced in the absence of catalyst and under mild conditions. In addition, the invention provides an industrial means for producing the compound, without using a large amount of an acid or a base serving as a reaction promoter or a catalyst, which would otherwise cause side reactions, apparatus corrosion, etc.

摘要翻译： 本发明提供一种制备由式（1）表示的苯并二氢吡喃化合物的方法，其特征在于该方法包括使苯酚，不饱和化合物和甲醛在不存在催化剂的情况下和在水存在下反应， 为摩尔比的1〜10倍。 根据本发明，可以在不存在催化剂的条件下，在温和的条件下生产高纯度色满化合物。 此外，本发明提供了一种用于生产化合物的工业方法，而不使用大量的酸或作为反应促进剂或催化剂的碱，否则会引起副反应，装置腐蚀等。

公开(公告)号：US20060167312A1

公开(公告)日：2006-07-27

申请号：US10563088

申请日：2004-07-01

申请人： Takafumi Yoshimura ,  Toshio Hidaka ,  Yoshifumi Sato ,  Norio Fushimi ,  Kazuhiro Yamada

发明人： Takafumi Yoshimura ,  Toshio Hidaka ,  Yoshifumi Sato ,  Norio Fushimi ,  Kazuhiro Yamada

IPC分类号： C07C63/04

CPC分类号： C07C51/363 ,  C07C63/70

摘要： The present invention provides a process for producing 5-iodo-2-methylbenzoic acid through iodination of 2-methylbenzoic acid, the process including, as essential steps, a reaction step of iodinating 2-methylbenzoic acid in the presence of a microporous compound, iodine, an oxidizing agent, and acetic anhydride, and a purification step including sublimation, distillation, crystallization, or a combination of two or more of these. According to the present invention, 5-iodo-2-methylbenzoic acid, which is useful for producing functional chemicals such as drugs, can be produced at high purity and high yield in a simple manner. Since the production process includes a simple reaction step and a simple separation/purification step, the load of purification is mitigated. In addition, the microporous compound such as a zeolite catalyst which has been separated and recovered from the reaction mixture can be repeatedly employed after performing of a simple treatment. Thus, the production process ensures a long service life of catalysts and high efficiency.

摘要翻译： 本发明提供了通过2-甲基苯甲酸碘化生产5-碘-2-甲基苯甲酸的方法，该方法包括作为必要步骤的步骤，在微孔化合物存在下碘化2-甲基苯甲酸，碘 ，氧化剂和乙酸酐，以及包括升华，蒸馏，结晶或这些中的两种或更多种的组合的纯化步骤。 根据本发明，可以以高纯度和高产率以简单的方式制备可用于制备功能性化学物质如药物的5-碘-2-甲基苯甲酸。 由于生产过程包括简单的反应步骤和简单的分离/纯化步骤，减轻了纯化负荷。 此外，在进行简单处理之后，可以重复使用从反应混合物中分离回收的微孔化合物如沸石催化剂。 因此，生产过程确保催化剂的使用寿命长，效率高。