公开(公告)号：US4918196A

公开(公告)日：1990-04-17

申请号：US831915

申请日：1986-02-21

申请人： Masaharu Doya ,  Toshio Kondo ,  Hideo Igarashi ,  Takako Uchiyama

发明人： Masaharu Doya ,  Toshio Kondo ,  Hideo Igarashi ,  Takako Uchiyama

IPC分类号： C07D233/72 ,  C12P13/04 ,  C12P41/00

CPC分类号： C12P41/006 ,  C12P13/04

摘要： A process for optically isomerizing an optically active alpha-amino acid amide comprising heating a D-alpha-amino acid amide or an L-alpha-amino acid amide in the presence of a strongly basic compound; and a process for producing an L-alpha-amino acid, which comprises(1) subjecting a D,L-alpha-amino acid amide or a mixture of a major amount of a D-alpha-amino acid amide and a minor amount of an L-alpha-amino acid amide to the action of a microorganism having the ability to hydrolyze the L-alpha-amino acid to obtain a hydrolyzate containing the L-alpha-amino acid and D-alpha-amino acid,(2) separating the L-alpha-amino acid from the hydrolyzate and recovering the remaining D-alpha-amino acid amide.(3) heating all or part of the recovered D-alpha-amino acid amide in the presence of a strongly basic substance to obtain a D,L-alpha-amino acid amide or a mixture of a major amount of the D-alpha-amino acid amide and a minor amount of the L-alpha-amino acid amide, and(4) recycling the D,L-alpha-amino acid amide or the mixture to step (1) as part or all of the starting material.

摘要翻译： 包括光学异构化光学活性α-氨基酸酰胺的方法，包括在强碱性化合物存在下加热D-α-氨基酸酰胺或L-α-氨基酸酰胺; 以及制备L-α-氨基酸的方法，其包括（1）使D，L-α-氨基酸酰胺或主要量的D-α-氨基酸酰胺和少量的 L-α-氨基酸酰胺，具有水解L-α-氨基酸的能力的微生物的作用，得到含有L-α-氨基酸和D-α-氨基酸的水解产物，（2）分离 来自水解产物的L-α-氨基酸并回收剩余的D-α-氨基酸酰胺。 （3）在强碱性物质存在下加热全部或部分回收的D-α-氨基酸酰胺，得到D，L-α-氨基酸酰胺或大量D-α-氨基酸酰胺的混合物， 氨基酸酰胺和少量的L-α-氨基酸酰胺，和（4）将D，L-α-氨基酸酰胺或混合物循环到步骤（1）中作为起始原料的一部分或全部。

公开(公告)号：US4605477A

公开(公告)日：1986-08-12

申请号：US704596

申请日：1985-02-25

申请人： Masaharu Doya ,  Toshio Kondo ,  Hideo Igarashi ,  Takako Uchiyama

发明人： Masaharu Doya ,  Toshio Kondo ,  Hideo Igarashi ,  Takako Uchiyama

IPC分类号： C07C319/28 ,  C07C67/00 ,  C07C227/00 ,  C07C227/40 ,  C07C229/02 ,  C07C313/00 ,  C07C323/58 ,  C12P13/04 ,  B01D13/02

CPC分类号： B01D61/44 ,  C12P13/04 ,  B01D2311/2623

摘要： An .alpha.-amino acid is effectively separated and recovered from an aqueous solution containing at least an .alpha.-amino acid and its corresponding .alpha.-amino acid amide by performing ion-exchange electrodialysis in the presence of ammonia. A reaction product liquid obtained by biochemical asymmetric hydrolysis of a D, L-.alpha.-amino acid is used preferably as the raw material aqueous solution for dialysis.

摘要翻译： 通过在氨的存在下进行离子交换电渗析，从含有至少α-氨基酸及其相应的α-氨基酰胺的水溶液中有效地分离和回收α-氨基酸。 优选使用通过D，L-α-氨基酸的生物化学不对称水解获得的反应产物作为用于透析的原料水溶液。

公开(公告)号：US06174711B1

公开(公告)日：2001-01-16

申请号：US09351619

申请日：1999-07-12

申请人： Akinori Tanaka ,  Masaharu Doya ,  Takako Uchiyama ,  Torakazu Tahara

发明人： Akinori Tanaka ,  Masaharu Doya ,  Takako Uchiyama ,  Torakazu Tahara

IPC分类号： C12P1306

CPC分类号： C07C237/06 ,  C07C231/10 ,  C07D317/30 ,  C07D319/06 ,  C12P41/006

摘要： A method for producing L-allysine acetal represented by general formula (II), comprising reacting D,L-allysinamide acetal represented by general formula (I) with cells of microorganism or treated cell product having an activity of stereoselectively hydrolyzing L-allysinamide acetal, wherein R1 and R2, which may be the same or different, each independently represent a lower alkyl group, or R1 and R2 are combined to form an alkylene group represented by [CH2]n, and n is 2 to 3. D,L-allysinamide acetal represented by general formula (I) is also in the scope of the invention. According to the present invention, L-allysine acetal useful as a raw material for medicine can be produced in a smaller number of steps at low costs.

摘要翻译： 一种由通式（II）表示的L-烯丙基乙缩醛的制备方法，其特征在于，将由通式（I）表示的D，L-烯丙基酰胺缩醛与具有立体选择性水解L-烯丙基酰胺缩醛活性的微生物或经处理的细胞产物反应， 其中R 1和R 2可以相同或不同，各自独立地表示低级烷基，或者R 1和R 2结合形成由[CH 2] n表示的亚烷基，n为2至3.D，L- 由通式（I）表示的烯丙基酰胺缩醛也在本发明的范围内。 根据本发明，可以低成本地以较少数量的步骤生产用作医药原料的L-烯丙基乙缩醛。

公开(公告)号：US4459423A

公开(公告)日：1984-07-10

申请号：US355142

申请日：1982-03-05

申请人： Masaharu Doya ,  Takako Uchiyama

发明人： Masaharu Doya ,  Takako Uchiyama

IPC分类号： C07C51/06

CPC分类号： C07C227/18 ,  C07C319/20

摘要： A process for producing efficiently and economically without using strong acids nor strong bases, .alpha.-amino acids from .alpha.-amino acid amides by hydrolyzing .alpha.-amino acid amides in an aqueous medium in the presence of ammonia. If necessary, the resultant hydrolyzate liquid from which .alpha.-amino acid has been removed may be reused.

摘要翻译： 在氨的存在下，通过在水性介质中水解α-氨基酸酰胺，而不使用强酸或强碱来从α-氨基酸酰胺生产α-氨基酸的方法。 如果需要，可以重复使用从其中除去α-氨基酸的所得水解液。

公开(公告)号：US5440004A

公开(公告)日：1995-08-08

申请号：US238743

申请日：1994-05-05

申请人： Masaharu Doya ,  Yutaka Kanbara ,  Ken-ichi Kimizuka ,  Takashi Okawa

发明人： Masaharu Doya ,  Yutaka Kanbara ,  Ken-ichi Kimizuka ,  Takashi Okawa

IPC分类号： C07D317/36 ,  C08G64/00

CPC分类号： C07D317/36

摘要： A method for the production of an alkylene carbonate at high yields and high selectivity by a reaction between an alkylene glycol and urea, the method being capable to preventing the deposition of a white crystal in the reflux condenser used in a conventional method for the production of alkylene carbonate and the subsequent decrease in the yield, wherein:a gas washing member and a cooling member are disposed above a reaction portion where alkylene glycol and urea are allowed to react,ammonia-containing steam exhausted from the reaction portion is downwardly introduced into the cooling member through the gas washing member,condensate and ammonia gas exhausted from a bottom of the cooling member are gas-liquid separated,the condensate is introduced into the gas washing member, andthe ammonia gas is removed from the reaction system.

摘要翻译： 一种通过亚烷基二醇和尿素之间的反应以高产率和高选择性生产碳酸亚烷基酯的方法，该方法能够防止白色结晶沉积在用于生产 碳酸亚烷基酯和随后的产率降低，其中：气体洗涤部件和冷却部件设置在使亚烷基二醇和尿素反应的反应部分上方，从反应部分排出的含氨蒸气被向下引入 通过气体洗涤部件的冷却部件，从冷却部件的底部排出的冷凝物和氨气体被气液分离，将冷凝物引入到气体洗涤部件中，从反应体系中除去氨气。

公开(公告)号：US07750182B2

公开(公告)日：2010-07-06

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 ,  C07C63/04

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：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：US4328374A

公开(公告)日：1982-05-04

申请号：US166114

申请日：1980-07-07

申请人： Shigeo Yoshinaka ,  Masaharu Doya

发明人： Shigeo Yoshinaka ,  Masaharu Doya

IPC分类号： C07C47/544 ,  C07C17/14 ,  C07C45/00 ,  C07C45/27 ,  C07C45/80 ,  C07C45/81 ,  C07C67/00 ,  C07C45/28

CPC分类号： C07C45/80 ,  C07C17/14 ,  C07C45/27 ,  C07C45/81

摘要： A process for the production of aromatic dialdehydes which comprises reacting xylene chloride selected from the group consisting of .alpha.,.alpha.,.alpha.'-trichloroxylene alone, or a mixture of .alpha.,.alpha.,.alpha.'-trichloroxylene and .alpha.,.alpha.'-dichloroxylene, a mixture of .alpha.,.alpha.,.alpha.'-trichloroxylene and .alpha.,.alpha.,.alpha.',.alpha.'-tetrachloroxylene and a mixture of .alpha.,.alpha.,.alpha.'-trichloroxylene, .alpha.,.alpha.'-dichloroxylene and .alpha.,.alpha.,.alpha.',.alpha.'-tetrachloroxylene with nitric acid.

摘要翻译： 一种制备芳族二醛的方法，其包括使选自α，α，α'-三氯代二氧化硅或单独的α，α，α'-三氯代二甲苯和α，α'-二氯二氧化硅的混合物的二甲苯氯反应， α，α，α'-三氯代二甲苯和α，α，α'，α'-四氯代二甲苯和α，α，α'-三氯代二甲苯，α，α'-二氯二氧化碳和α，α，α'，α ' - 四氯二氧化硅与硝酸。

公开(公告)号：US4165337A

公开(公告)日：1979-08-21

申请号：US844814

申请日：1977-10-25

申请人： Shigeo Yoshinaka ,  Masaharu Doya ,  Seiji Uchiyama ,  Sadao Nozaki

发明人： Shigeo Yoshinaka ,  Masaharu Doya ,  Seiji Uchiyama ,  Sadao Nozaki

IPC分类号： C07C63/15 ,  B01J19/12 ,  C07C17/14 ,  C07C51/00 ,  C07C51/60 ,  C07C67/00 ,  C07C51/58

CPC分类号： C07C17/14 ,  C07C51/60

摘要： A batchwise or continuous process for producing isophthaloyl dichloride or terephthaloyl dichloride having a high purity which comprises, in combination, (1) a first step of producing .alpha.,.alpha.,.alpha.,.alpha.',.alpha.',.alpha.'-hexachloroxylene by reacting meta- or para-xylene with chlorine under the irradiation of ultraviolet-containing rays, the reaction being carried out in the presence of, as a solvent, .alpha.,.alpha.,.alpha.,.alpha.',.alpha.',.alpha.'-hexachloroxylene added at the outset of the reaction; (2) a second step of producing isophthaloyl dichloride or terephthaloyl dichloride by reacting the .alpha.,.alpha.,.alpha.,.alpha.',.alpha.',.alpha.'-hexachloroxylene obtained in the first step with isophthalic acid or terephthalic acid; and (3) a third step of purifying the isophthaloyl dichloride or terephthaloyl dichloride obtained in the second step by dissolving the isophthaloyl dichloride or terephthaloyl dichloride in 0.3 to 6 parts by weight; per part by weight of the phthaloyl dichloride, of C.sub.6 -C.sub.10 aliphatic hydrocarbon solvent, and cooling the solution to a temperature of the specified range thereby to recrystallize the phthaloyl dichloride.

摘要翻译： 用于制备具有高纯度的间苯二酰二氯或对苯二甲酰氯的间歇或连续方法，其组合包括（1）通过使间位化合物反应生成α，α，α，α'，α'，α'-六氯代二甲苯的第一步骤， 或对二甲苯与氯在紫外线照射下反应，反应在作为溶剂的存在下进行，α，α，α，α'，α'，α'-六氯化碳在开始时加入 反应; （2）通过使第一步获得的α，α，α，α'，α'，α'-六氯二苯与间苯二甲酸或对苯二甲酸反应，生产间苯二酰二氯或对苯二甲酰氯的第二步; 和（3）通过将间苯二酰二氯或对苯二酰氯溶解在0.3至6重量份中来纯化在第二步中获得的间苯二酰二氯或对苯二甲酰氯的第三步骤; 每重量份邻苯二甲酰二氯化物，C 6 -C 10脂族烃溶剂，并将溶液冷却至指定范围的温度，从而使邻苯二甲酰氯二氯化物重结晶。

公开(公告)号：US20110172465A1

公开(公告)日：2011-07-14

申请号：US13063541

申请日：2009-03-27

申请人： Masaharu Doya

发明人： Masaharu Doya

IPC分类号： C07C45/61

CPC分类号： C07B53/00 ,  B01J23/02 ,  B01J23/06 ,  B01J31/1805 ,  B01J31/2452 ,  B01J2531/0266 ,  B01J2531/821 ,  C07C45/62 ,  C07C45/74 ,  C07C45/82 ,  C07C49/385 ,  C07C49/587

摘要： By intramolecular condensation reaction of 2,15-hexadecanedione in a gaseous phase with a compound of a Group II element of the Periodic Table as a catalyst, 3-methyl-cyclopentadecenones is generated. Magnesium oxide, calcium oxide, or zinc oxide is desirable as the catalyst for the intramolecular condensation reaction. (R)- and (S)-muscone is generated by subjecting 3-methyl-cyclopentadecenones obtained as above to hydrogenation by using a catalyst. Palladium catalyst is desirable as the hydrogenation catalyst. Optically active muscone is generated by separating 3-methyl-cyclopentadecenones into respective components thereof by means of precision distillation and subsequently subjecting the separated 3-methyl-cyclopentadecenones to asymmetric hydrogenation by using an optically active ruthenium complex catalyst. The production methods described above enable easy and economical production of 3-methyl-cyclopentadecenones, (R)- and (S)-muscone, and optically active muscone.

摘要翻译： 通过将气相中的2,15-十六烷二酮与周期表的II族元素的化合物作为催化剂的分子内缩合反应，产生3-甲基 - 环戊烯酮。 作为分子内缩合反应的催化剂，优选氧化镁，氧化钙或氧化锌。 通过使用上述得到的3-甲基 - 环十五烯酮通过使用催化剂进行氢化而生成（R） - 和（S） - 壳多糖。 作为氢化催化剂，钯催化剂是理想的。 通过精密蒸馏将3-甲基 - 环十五烯酮分成其各自的组分，然后通过使用光学活性钌络合物催化剂将分离的3-甲基 - 环十五烯酮进行不对称氢化，产生光学活性的肌肉。 上述制造方法能够容易且经济地生产3-甲基 - 环戊烯酮，（R） - 和（S） - 软骨素和光学活性的肌肉。