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1. 发明申请

US20230127147A1 CONTINUOUS-FLOW PREPARATION METHOD OF DIOL SULFONE 有权
公开(公告)号：US20230127147A1
公开(公告)日：2023-04-27
申请号：US18068151
申请日：2022-12-19
申请人： Fudan University
发明人： Fener CHEN , Minjie LIU , Meifen JIANG , Yingqi XIA , Huashan HUANG
IPC分类号： C07C315/02 , C07C315/06
摘要： A continuous-flow preparation method of diol sulfone using a two-stage micro-reaction system. The system includes a first micro-mixer, a first micro-channel reactor, a second micro-mixer, and a second micro-channel reactor communicated in sequence. The method includes: feeding hydrogen peroxide, a catalyst and a diol thioether solution simultaneously to the first micro-mixer followed by mixing; feeding the reaction mixture to the first micro-channel reactor for continuous oxidation; and feeding the reaction mixture and water simultaneously to the second micro-mixer and the second micro-channel reactor for continuous quenching and crystallization to obtain diol sulfone.

2. 发明申请

US20230054928A1 METHOD FOR PREPARING CARBONYL SULFONE 有权
公开(公告)号：US20230054928A1
公开(公告)日：2023-02-23
申请号：US17780699
申请日：2020-11-27
申请人： SOOCHOW UNIVERSITY
发明人： Xiaobing WAN , Hanghang WANG , Yonggao ZHENG , Pengcheng LIAN , Jingjing LI
IPC分类号： C07C315/02 , C07C315/06
摘要： Disclosed is a method for preparing β-carbonyl sulfones. The method comprises: by taking an α-carbonyl diazo compound and sodium arylsulfinate as reaction substrates, cheap silver nitrate as an optimal catalyst, 1,10-phenanthroline as a ligand, and potassium persulfate as an oxidant, carrying out coupling reaction in a mixed solvent of acetonitrile and water to obtain a β-carbonyl sulfones compound. Compared with the prior art, the method has the following advantages: a wide range of reaction substrates, short reaction time, a relatively high reaction yield, a mild reaction condition, etc. In the present invention, non-toxic and harmless reagents are used as reaction raw materials, so that it has no harm to the environment and satisfies the requirements of contemporary green chemistry development. Post-reaction treatment is relatively simple, and is convenient for separation and purification. In addition, the reaction can achieve gram-scale synthesis, and lays a foundation for actual applications.

3. 发明申请

US20220098147A1 PROCESS FOR PRODUCING 4,4`-DICHLORODIPHENYL SULFOXIDE 有权
公开(公告)号：US20220098147A1
公开(公告)日：2022-03-31
申请号：US17429210
申请日：2020-02-06
申请人： BASF SE
发明人： Jun GAO , Indre THIEL , Christian SCHUETZ , Lukas METZGEN , Oliver BEY , Stefan BLEI
IPC分类号： C07C315/02 , C07C315/06
摘要： The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfoxide comprising: (I) reacting thionyl chloride, chlorobenzene and aluminum chloride in a molar ratio of thionyl chloride:chlorobenzene:aluminum chloride of 1:(6 to 9):(1 to 1.5) at a temperature in the range from 0 to below 20° C., forming an intermediate reaction product and hydrogen chloride; (II) mixing aqueous hydrochloric acid and the intermediate reaction product at a temperature in the range from 70 to 110° C. to obtain an organic phase comprising 4,4′-dichlorodiphenyl sulfoxide and an aqueous phase; (III) cooling the organic phase comprising the 4,4′-dichlorodiphenyl sulfoxide to a temperature below the saturation point of 4,4′-dichlorodiphenyl sulfoxide to obtain a suspension comprising crystallized 4,4′-dichlorodiphenyl sulfoxide; (IV) solid-liquid-separation of the suspension to obtain a residual moisture containing solid 4,4′-dichlorodiphenyl sulfoxide comprising crystallized 4,4′-dichlorodiphenyl sulfoxide and mother liquor.

4. 发明授权

US11028047B2 Method for recovering dimethyl sulfoxide from recovered resist remover 有权
公开(公告)号：US11028047B2
公开(公告)日：2021-06-08
申请号：US16630630
申请日：2018-07-31
申请人： KURARAY CO., LTD.
发明人： Kunio Mayahara , Koji Tamura , Akinobu Takeda
IPC分类号： B01D3/34 , C07C315/06 , C07C29/80
摘要： A method for recovering dimethyl sulfoxide, including a step of contacting a recovered resist remover containing at least one compound selected from the group consisting of glycol ether, glycol and triol, and dimethyl sulfoxide with water and performing distillation.

5. 发明申请

US20210121422A1 GLUCAGON RECEPTOR ANTAGONISTS 有权
公开(公告)号：US20210121422A1
公开(公告)日：2021-04-29
申请号：US16969521
申请日：2019-02-13
申请人： LIGAND PHARMACEUTICALS INCORPORATED , METAVANT SCIENCES GMBH
发明人： Lin Zhi , Ian Henderson , Joseph Kaloko , Martin Osterhout
IPC分类号： A61K31/185 , C07C309/24 , A61K31/155 , A61K31/427 , A61K31/4439 , A61K38/28 , A61K38/31 , A61K31/7032 , A61K31/702 , A61K31/64 , A61K31/366 , A61K31/455 , A61K45/06 , C07C315/04 , C07C201/12 , C07C209/36 , C07C67/343 , C07C67/00 , C07C231/02 , C07C231/12 , C07C315/06
摘要： Provided herein are solid state forms of compounds, including enantiomerically pure forms thereof, and pharmaceutically acceptable salts or co-crystals and prodrugs thereof which have glucagon receptor antagonist or inverse agonist activity. Further, provided herein are pharmaceutical compositions and methods of treating, preventing, ameliorating, delaying the time to onset or reducing the risk for the development or progression of at least one condition, disease, or disorder for which one or more glucagon receptor antagonist is indicated, including Type I and II diabetes, insulin resistance, hyperglycemia, ketoacidosis, or ketosis.

6. 发明授权

US10899705B2 Process for the manufacturing of methane sulfonic acid 有权
公开(公告)号：US10899705B2
公开(公告)日：2021-01-26
申请号：US16614599
申请日：2018-05-23
申请人： BASF SE
发明人： Jan Spielmann , Michael Zeilinger , Juergen Wortmann , Frieder Borgmeier
IPC分类号： C07C317/04 , C07C315/06 , C07C303/06 , C07C303/44 , C07C309/04
摘要： The present invention relates to a process for the manufacturing of methane sulfonic acid (MSA) by reaction of a radical initiator composition with methane and sulfur trioxide comprising the steps (a) preparation of the intiator composition by reacting aqueous hydrogen peroxide with the components methane sulfonic acid and methane sulfonic acid anhydride and (b) reaction of the initiator composition from step (a) with sulfur trioxide and methane to form methane sulfonic acid. The invention further relates to the use of methane sulfonic acid anhydride (MSA anhydride) in said process and to methane sulfonic acid manufactured by said process.

7. 发明授权

US07619120B2 Processes for the preparation of diphenylsulfone compounds 有权
标题翻译：二苯砜化合物的制备方法
公开(公告)号：US07619120B2
公开(公告)日：2009-11-17
申请号：US10950889
申请日：2004-09-27
申请人： Kiyoshi Katsuura , Tomoya Hidaka , Yutaka Takashina , Yasuo Ohnuki
发明人： Kiyoshi Katsuura , Tomoya Hidaka , Yutaka Takashina , Yasuo Ohnuki
IPC分类号： C07C315/06
CPC分类号： C07C315/04 , C07C315/06 , C07C317/22
摘要： The present invention is to provide methods for producing highly pure 4,4′-dihydroxydiphenyl sulfone monoethers advantageously in industrial production.In a process for producing a compound represented by Formula (I) (wherein, R1 and R2 are each independently halogen, alkyl having 1 to 8 carbons or alkenyl having 2 to 8 carbons; m and n are each independently 0 or an integer of 1 to 4; and R3 is alkyl having 1 to 8 carbons, alkenyl having 2 to 8 carbons, cycloalkyl having 3 to 8 carbons or optionally substituted aralkyl), (1) a pH adjustment is carried out twice or more in the purification process, (2) an excessive amount of alkyl halide used is removed, (3) a solvent, such as water, containing 0.05 ppm or less of iron components is used, (4) tanks with corrosion-resistant layers over the inner walls are used, (6) a chelating agent is added, and (7) a means of drying with mechanical stir is applied.
摘要翻译：本发明提供在工业生产中有利地生产高纯度4,4'-二羟基二苯砜单醚的方法。在制备由式（I）表示的化合物的方法中（其中，R 1和R 2各自独立地为卤素，具有1至8个碳的烷基或具有2至8个碳的烯基; m和n各自独立地为0或整数1 至4; R3为具有1至8个碳的烷基，具有2至8个碳的烯基，3至8个碳原子的环烷基或任选取代的芳烷基），（1）在纯化过程中进行两次或更多次的pH调节（ 2）除去过量的烷基卤，（3）使用含有0.05ppm以下铁组分的溶剂如水，（4）使用内壁上具有耐腐蚀层的罐（ 6）加入螯合剂，（7）用机械搅拌干燥的方法。

8. 发明申请

US20080045751A1 Process for Purifying Mesotrione 有权
标题翻译：净化中草酮的方法
公开(公告)号：US20080045751A1
公开(公告)日：2008-02-21
申请号：US10573723
申请日：2004-10-01
申请人： Julie Marie Wichert , Alan Henry Benke , Regine Laure Guidetti-Grep
发明人： Julie Marie Wichert , Alan Henry Benke , Regine Laure Guidetti-Grep
IPC分类号： C07C315/06 , C07C317/24
CPC分类号： C07C315/04 , C07C315/06 , C07C317/24
摘要： A process for reducing the levels of undesirable impurities in a mesotrione sample is disclosed, said process comprising the steps of:(i) forming a mesotrione enolate solution in an aqueous solvent,(ii) carrying out one or more purification processes, and(iii) crystallising the purified mesotrione out of solution.
摘要翻译：公开了一种用于降低甲基异硫脲样品中不希望的杂质水平的方法，所述方法包括以下步骤：（i）在水性溶剂中形成甲基磺酸烯醇酯溶液，（ii）进行一种或多种纯化方法，和（iii ）将纯化的甲磺草酮从溶液中结晶。

9. 发明授权

US07285678B2 Purification of 2-nitro-4-methylsulphonylbenzoic acid 有权
标题翻译： 2-硝基-4-甲基磺酰基苯甲酸的纯化
公开(公告)号：US07285678B2
公开(公告)日：2007-10-23
申请号：US10472962
申请日：2002-03-25
申请人： Kambiz Javdani , Gilbert Rodriguez , James Peter Muxworthy
发明人： Kambiz Javdani , Gilbert Rodriguez , James Peter Muxworthy
IPC分类号： C07C315/06
CPC分类号： C07C315/06 , C07C317/44
摘要： A method for removing impurities from 2-nitro-4-methylsulfonylbenzoic acid which comprises at least two of the following steps, in any order, (a) dissolving 2-nitro-4-methylsulfonylbenzoic acid in water at a pH of about 2 to 10, followed by filtration; (b) contacting an aqueous solution of 2-nitro-4-methylsulfonylbenizoic acid with activated carbon at a pH of about 2 to 10; (c) treating an aqueous solution of 2-nitro-4-methylsulfonylbenzoic acid with sufficient base to hydrolyze undesired nitro and dinitro substituted impurities; followed by maintaining the resulting aqueous solution comprising 2-nitro-4-methylsulfonylbenzoic acid at a temperature of up to about 95° C., and adjusting the pH of said solution to about a pH which is sufficient to effect crystallization of 2-nitro-4-methylsulfonylbenzoic acid upon cooling.
摘要翻译：一种从2-硝基-4-甲基磺酰基苯甲酸中除去杂质的方法，该方法包括至少两个以下步骤，以任何顺序，（a）将2-硝基-4-甲基磺酰基苯甲酸溶于约2至10的pH下的水中，然后过滤; （b）将2-硝基-4-甲基磺酰基二十八碳酸的水溶液与约2至10的pH下的活性炭接触; （c）用足够的碱处理2-硝基-4-甲基磺酰基苯甲酸的水溶液以水解不希望的硝基和二硝基取代的杂质; 然后将所得到的包含2-硝基-4-甲基磺酰基苯甲酸的水溶液在高至约95℃的温度下保持，并将所述溶液的pH调节至足以使2-硝基-4-甲基磺酰基苯甲酸结晶的pH值， 4-甲基磺酰基苯甲酸。

10. 发明授权

US07189880B2 Process for producing 2,4′-dihydroxydiphenylsulfone 有权
标题翻译： 2,4'-二羟基二苯砜的制备方法
公开(公告)号：US07189880B2
公开(公告)日：2007-03-13
申请号：US10500997
申请日：2003-01-22
申请人： Gou Yoshino , Yuichi Tomoda , Norihiro Taniguchi , Kazuaki Igarashi , Takeo Hasegawa
发明人： Gou Yoshino , Yuichi Tomoda , Norihiro Taniguchi , Kazuaki Igarashi , Takeo Hasegawa
IPC分类号： C07C315/06 , C07C315/00
CPC分类号： C07C315/04 , C07C315/06 , C07C317/22
摘要： A process for producing 2,4′-dihydroxydiphenylsulfone which comprises separating 4,4′-dihydroxydiphenylsulfone by crystallization from a mixture containing 4,4′-dihydroxydiphenylsulfone, 2,4′-dihydroxydiphenylsulfone, phenolsulfonic acid and phenol which is obtained by dehydration of phenol and sulfuric acid or phenolsulfonic acid to obtain a mixture having a content of 2,4′-dihydroxydiphenylsulfone greater than the content of 4,4′-dihydroxydiphenylsulfone, crystallizing 2,4′-dihydroxydiphenylsulfone by adjusting the composition of the solvent of the obtained mixture so that the ratio of the amounts by weight of phenol to water is 10:90 to 90:10, and separating 2,4′-dihydroxydiphenylsulfone by filtration; and a process as described above in which the filtrate obtained by the filtration is used as the raw material for the hydration.
摘要翻译：一种2,4'-二羟基二苯砜的制备方法，其包括通过结晶从4,4'-二羟基二苯基砜，2,4'-二羟基二苯基砜，苯酚磺酸和苯酚的混合物中分离出4,4'-二羟基二苯基砜，其通过苯酚脱水得到和硫酸或苯酚磺酸，得到含量大于4,4'-二羟基二苯砜含量的2,4'-二羟基二苯砜的混合物，通过调节所得混合物的溶剂组成使2,4'-二羟基二苯砜结晶使苯酚与水的重量比为10:90〜90:10，过滤分离2,4'-二羟基二苯砜; 和通过过滤获得的滤液用作水合原料的上述方法。

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