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    • 1. 发明授权
    • Method and apparatus for the production of alkylene carbonate
    • 用于生产碳酸亚烷基酯的方法和装置
    • US5440004A
    • 1995-08-08
    • US238743
    • 1994-05-05
    • Masaharu DoyaYutaka KanbaraKen-ichi KimizukaTakashi Okawa
    • Masaharu DoyaYutaka KanbaraKen-ichi KimizukaTakashi Okawa
    • C07D317/36C08G64/00
    • C07D317/36
    • 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.
    • 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。
    • 2. 发明授权
    • Process for recimization of an optically active alpha-amino acid amides
and process for producing optically active alpha-amino acids
    • 用于重新获得光学活性α-氨基酸酰胺的方法和用于制备光学活性α-氨基酸的方法
    • US4918196A
    • 1990-04-17
    • US831915
    • 1986-02-21
    • Masaharu DoyaToshio KondoHideo IgarashiTakako Uchiyama
    • Masaharu DoyaToshio KondoHideo IgarashiTakako Uchiyama
    • C07D233/72C12P13/04C12P41/00
    • C12P41/006C12P13/04
    • 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.
    • 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。
    • 3. 发明授权
    • Process for production of iodine compounds and process for production of high-purity 5-iodo-2-methylbenzoic acid
    • 生产碘化合物的方法和生产高纯度5-碘-2-甲基苯甲酸的方法
    • US07750182B2
    • 2010-07-06
    • US10545005
    • 2004-02-10
    • Toshio HidakaTakafumi YoshimuraYoshifumi SatoNorio FushimiMasaharu Doya
    • Toshio HidakaTakafumi YoshimuraYoshifumi SatoNorio FushimiMasaharu Doya
    • C07C17/00C07C63/04
    • C07C253/30C07B39/00C07C17/12C07C17/156C07C17/158C07C51/363C07C51/43C07C25/02C07C25/13C07C25/18C07C25/125C07C63/70C07C255/50
    • 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.
    • 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。
    • 4. 发明申请
    • Process for production of iodine compounds and process for production of high-purity 5-iodo-2-methylbenzoic acid
    • 生产碘化合物的方法和生产高纯度5-碘-2-甲基苯甲酸的方法
    • US20060161028A1
    • 2006-07-20
    • US10545005
    • 2004-02-10
    • Toshio HidakaTakafumi YoshimuraYoshifumi SatoNorio FushimiMasaharu Doya
    • Toshio HidakaTakafumi YoshimuraYoshifumi SatoNorio FushimiMasaharu Doya
    • C07C17/00
    • C07C253/30C07B39/00C07C17/12C07C17/156C07C17/158C07C51/363C07C51/43C07C25/02C07C25/13C07C25/18C07C25/125C07C63/70C07C255/50
    • 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.
    • 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。
    • 8. 发明授权
    • Process for producing phthaloyl dichlorides of high purity
    • 生产高纯度邻苯二甲酰氯的方法
    • US4165337A
    • 1979-08-21
    • US844814
    • 1977-10-25
    • Shigeo YoshinakaMasaharu DoyaSeiji UchiyamaSadao Nozaki
    • Shigeo YoshinakaMasaharu DoyaSeiji UchiyamaSadao Nozaki
    • C07C63/15B01J19/12C07C17/14C07C51/00C07C51/60C07C67/00C07C51/58
    • C07C17/14C07C51/60
    • 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.
    • 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。
    • 9. 发明申请
    • METHOD FOR PRODUCING 3-METHYL-CYCLOPENTADECENONES, METHOD FOR PRODUCING (R)- AND (S)- MUSCONE, AND METHOD FOR PRODUCING OPTICALLY ACTIVE MUSCONE
    • 用于生产3-甲基环戊二烯的方法,用于生产(S) - 和(S) - 马铃薯的方法,以及用于生产光学活性麦克风的方法
    • US20110172465A1
    • 2011-07-14
    • US13063541
    • 2009-03-27
    • Masaharu Doya
    • Masaharu Doya
    • C07C45/61
    • C07B53/00B01J23/02B01J23/06B01J31/1805B01J31/2452B01J2531/0266B01J2531/821C07C45/62C07C45/74C07C45/82C07C49/385C07C49/587
    • 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.
    • 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。