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1. 发明授权

US6031108A Process for the preparation of 2-(methylsulfonyl)-5-(trifluoromethyl)-1,3,4-thiadiazole (TDA sulfone) 有权
标题翻译：制备2-（甲基磺酰基）-5-（三氟甲基）-1,3,4-噻二唑（TDA砜）的方法
公开(公告)号：US6031108A
公开(公告)日：2000-02-29
申请号：US153920
申请日：1998-09-16
申请人： Vidyanatha A. Prasad , Klaus Jelich , Joe J. Hanson
发明人： Vidyanatha A. Prasad , Klaus Jelich , Joe J. Hanson
IPC分类号： B01J31/34 , C07B61/00 , C07D285/12 , C07D285/125
CPC分类号： C07D285/125
摘要： The present invention provides a process for making thiadiazole sulfones. In particular, the present process is used to make 2-(methylsulfonyl)-5-(trifluoromethyl)-1,3,4-thiadiazole using catalytic oxidation in the presence of a suitable oxidizing agent. The catalyst system used for the oxidation reaction is a mixture of glacial acetic acid and a tungsten catalyst. The tungsten catalyst is preferably selected from the group consisting of sodium tungstate, potassium tunstate, and tungstic acid.
摘要翻译：本发明提供了制备噻二唑砜的方法。特别地，本方法用于在合适的氧化剂存在下使用催化氧化制备2-（甲基磺酰基）-5-（三氟甲基）-1,3,4-噻二唑。用于氧化反应的催化剂体系是冰醋酸和钨催化剂的混合物。钨催化剂优选选自钨酸钠，焦磷酸钾和钨酸。

2. 发明授权

US5965737A Approach to the conversion of 2-(methylthio)-5-(trifluoromethyl)-1,3,4-thiadiazole (TDA) to 2-(methylsulfonyl)-5-(trifluoromethyl)-1,3,4-thiadiazole (TDA sulfone) 失效
标题翻译：方法将2-（甲硫基）-5-（三氟甲基）-1,3,4-噻二唑（TDA）转化为2-（甲基磺酰基）-5-（三氟甲基）-1,3,4-噻二唑（TDA砜）
公开(公告)号：US5965737A
公开(公告)日：1999-10-12
申请号：US251571
申请日：1999-02-17
申请人： Vidyanatha A. Prasad , Joe J. Hanson , Klaus Jelich
发明人： Vidyanatha A. Prasad , Joe J. Hanson , Klaus Jelich
IPC分类号： C07D285/12 , C07D285/125
CPC分类号： C07D285/125
摘要： The present invention provides a process for making thiadiazole sulfones. In particular, the present process is used to make 2-(methyl-sulfonyl)-5-(trifluoromethyl)-1,3,4-thiadiazole using catalytic oxidation in the presence of a suitable oxidizing agent. A preferred oxidizing agent is hydrogen peroxide. The catalyst system used for the oxidation reaction is a mixture of boric acid and glacial acetic acid. The molar ratio of glacial acetic acid to 2-(methylthio)-5-(trifluoromethyl)-1,3,4-thiadiazole is from about 0.1:1 to about 0.5:1.
摘要翻译：本发明提供了制备噻二唑砜的方法。特别地，本方法用于在合适的氧化剂存在下使用催化氧化制备2-（甲基 - 磺酰基）-5-（三氟甲基）-1,3,4-噻二唑。优选的氧化剂是过氧化氢。用于氧化反应的催化剂体系是硼酸和冰醋酸的混合物。冰醋酸与2-（甲硫基）-5-（三氟甲基）-1,3,4-噻二唑的摩尔比为约0.1:1至约0.5:1。

3. 发明授权

US6147222A Process for the manufacture of sulfonylaminocarbonyl triazolinones and salts thereof under pH controlled conditions 有权
标题翻译：在pH控制条件下制备磺酰氨基羰基三唑啉酮及其盐的方法
公开(公告)号：US6147222A
公开(公告)日：2000-11-14
申请号：US472672
申请日：1999-12-27
申请人： Vidyanatha A. Prasad , Klaus Jelich
发明人： Vidyanatha A. Prasad , Klaus Jelich
IPC分类号： C07D249/12
CPC分类号： C07D249/12
摘要： The present invention relates to a process for manufacturing sulfonylaminocarbonyl triazolinones and salts thereof, which are herbicidally active compounds, wherein the improvement comprises conducting the conversion reaction of the sulfonylaminocarbonyl triazolinone to a salt thereof under pH controlled conditions. In particular, this invention relates to the conversion of a substituted triazolinone to a sulfonylaminocarbonyl triazolinone, and without the isolation of this intermediate product, the sulfonylaminocarbonyl triazolinone is then converted to a salt thereof.
摘要翻译：本发明涉及作为除草活性化合物的磺酰基氨基羰基三唑啉酮及其盐的制备方法，其中改进包括在pH控制条件下进行磺酰氨基羰基三唑啉酮与其盐的转化反应。特别地，本发明涉及取代的三唑啉酮转化为磺酰基氨基羰基三唑啉酮，并且不分离该中间产物，然后将磺酰基氨基羰基三唑啉酮转化为其盐。

4. 发明授权

US6075157A Purification of O,S-dimethyl phosphoramidothioate 失效
标题翻译： O，S-二甲基氨基硫代磷酸酯的纯化
公开(公告)号：US6075157A
公开(公告)日：2000-06-13
申请号：US134971
申请日：1998-08-17
申请人： Vidyanatha A. Prasad , Klaus Jelich
发明人： Vidyanatha A. Prasad , Klaus Jelich
IPC分类号： C07F9/02 , C07F9/24
CPC分类号： C07F9/025 , C07F9/2408
摘要： The present invention provides a method for making O,S-dimethyl phosphoramidothioate. In accordance with this process, O,O-dimethyl phosphoramidothioate is isomerized in the presence of dimethyl sulfate to form a reaction mixture; the reaction mixture is then passed through a wiped film evaporator at a temperature of from about 55.degree. C. to about 120.degree. C. and a pressure of from about 3 to about 10 mm Hg, with the distillate containing O,S-dimethyl phosphoramidothioate, unreacted O,O-dimethyl phosphoramidothioate and by-products, and the residue containing O,S-dimethyl phosphoramidothioate in an amount greater than the amount of O,S-dimethyl phosphoramidothioate contained in the reaction mixture prior to distillation.
摘要翻译：本发明提供了制备O，S-二甲基氨基硫代磷酸酯的方法。按照该方法，在硫酸二甲酯的存在下将O，O-二甲基硫代磷酸酯异构化，形成反应混合物; 然后将反应混合物在约55℃至约120℃的温度和约3至约10mm Hg的压力下通过刮膜蒸发器，馏出物含有O，S-二甲基氨基硫代磷酸酯，未反应的O，O-二甲基氨基硫代磷酸酯和副产物，以及含有大于O蒸馏前反应混合物中的O，S-二甲基氨基硫代磷酸酯的量的O，S-二甲基硫代磷酸酯的残余物。

5. 发明授权

US5922896A Process for making O,S-dimethyl phosphoramidothioate 失效
标题翻译：制备O，S-二甲基氨基硫代磷酸酯的方法
公开(公告)号：US5922896A
公开(公告)日：1999-07-13
申请号：US988302
申请日：1997-12-10
申请人： Vidyanatha A. Prasad , Klaus Jelich , Donald K. Smith
发明人： Vidyanatha A. Prasad , Klaus Jelich , Donald K. Smith
IPC分类号： C07F9/24
CPC分类号： C07F9/2408
摘要： The present invention provides a method for making O,S-dimethyl phosphoramidothioate. In accordance with the present process, O,O-dimethyl phosphoramidothioate is isomerized in the presence of a catalyst at a temperature of from about 35.degree. C. to about 45.degree. C. to form a mixture containing O,S-dimethyl phosphoramidothioate and the resultant mixture is lagered at a temperature of from about 35.degree. C. to about 45.degree. C. for about 3 to 6 hours. The total time for both steps is at least about 4 hours.
摘要翻译：本发明提供了制备O，S-二甲基氨基硫代磷酸酯的方法。根据本发明方法，在约35℃至约45℃的温度下，在催化剂存在下将O，O-二甲基硫代磷酸酯异构化，形成含有O，S-二甲基氨基硫代磷酸酯和所得混合物在约35℃至约45℃的温度下放置约3至6小时。两个步骤的总时间至少约4小时。

6. 发明授权

US5922404A Process for producing dimethyl (2,2,2-trichloro-1-hydroxyethyl)-phosphonate and granular formulations thereof 失效
标题翻译：二（2,2,2-三氯-1-羟乙基）膦酸二甲酯及其颗粒制剂的制备方法
公开(公告)号：US5922404A
公开(公告)日：1999-07-13
申请号：US939826
申请日：1997-09-29
申请人： Vidyanatha A. Prasad , Klaus Jelich , Christopher M. Tusa , Daniel E. Terry , Stephen C. Slahck , Scott P. Hensley
发明人： Vidyanatha A. Prasad , Klaus Jelich , Christopher M. Tusa , Daniel E. Terry , Stephen C. Slahck , Scott P. Hensley
IPC分类号： A01N57/20 , C07F9/40 , B05D7/00 , A61K31/66
CPC分类号： C07F9/4006 , A01N57/20 , Y02P20/125
摘要： The present invention relates to an integrated process for synthesizing dimethyl (2,2,2-trichloro-1-hydroxyethyl)-phosphonate and a process for impregnating the dimethyl (2,2,2-trichloro-1-hydroxyethyl)-phosphonate on to inert carrier granules. The process involves adding dimethyl phosphite to a reaction mixture containing chloral under anhydrous, inert conditions. The molar ratio of chloral to dimethyl phosphite used in the reaction mixture is from about 1.0:1.0 to about 1.1:1.0. The impregnation process involves transferring molten dimethyl (2,2,2-trichloro-1-hydroxyethyl)-phosphonate into a process vessel and discharging weighed aliquots into a formulation vessel to form a granular product containing dimethyl (2,2,2-trichloro-1-hydroxyethyl)-phosphonate.
摘要翻译：本发明涉及一种合成二甲基（2,2,2-三氯-1-羟基乙基）膦酸酯的方法和将二（2,2,2-三氯-1-羟基乙基）膦酸二甲酯浸渍在惰性载体颗粒。该方法包括在无水惰性条件下将亚磷酸二甲酯加入到含有氯醛的反应混合物中。在反应混合物中使用的氯醛与亚磷酸二甲酯的摩尔比为约1.0:1.0至约1.1:1.0。浸渍过程包括将熔融的二甲基（2,2,2-三氯-1-羟乙基）膦酸酯转移到处理容器中，并将重质等分试样排入制剂容器中以形成含有二甲基（2,2,2-三氯-1-羟乙基） 1-羟乙基） - 膦酸酯。

7. 发明授权

US06197971B1 Process for the manufacture of substituted triazolinones 有权
标题翻译：制备取代的三唑啉酮的方法
公开(公告)号：US06197971B1
公开(公告)日：2001-03-06
申请号：US09472482
申请日：1999-12-27
申请人： Shekhar V. Kulkarni , Vidyanatha A. Prasad , Vijay C. Desai , Eric Rivadeneira , Klaus Jelich
发明人： Shekhar V. Kulkarni , Vidyanatha A. Prasad , Vijay C. Desai , Eric Rivadeneira , Klaus Jelich
IPC分类号： C07D24912
CPC分类号： C07D249/12
摘要： The present invention relates to a process for manufacturing substituted triazolinones, which are intermediates in the preparation of herbicidally active compounds. In particular, this invention relates to the alkylation of a non-alkylated triazolinone intermediate product, wherein the improvement comprises conducting the alkylation reaction under pH controlled conditions. In a preferred embodiment, the invention relates to the preparation of a 5-alkoxy(or aryloxy)-2,4-dihydro-3H-1,2,4-triazol-3-one, and the alkylation of this non-alkylated triazolinone intermediate product, to produce a 5-alkoxy(or aryloxy)-4-alkyl-2,4-dihydro-3H-1,2,4-triazol-3-one.
摘要翻译：本发明涉及一种制备取代三唑啉酮的方法，它是制备除草活性化合物的中间体。特别地，本发明涉及非烷基化三唑啉酮中间产物的烷基化，其中改进包括在pH控制条件下进行烷基化反应。在优选的实施方案中，本发明涉及5-烷氧基（或芳氧基）-2,4-二氢-3H-1,2,4-三唑-3-酮的制备，并且该非烷基化的三唑啉酮的烷基化中间产物，生成5-烷氧基（或芳氧基）-4-烷基-2,4-二氢-3H-1,2,4-三唑-3-酮。

8. 发明授权

US5792872A Process for producing N-(4-fluorophenyl)-N-(1-methylethyl)-2-�(5-trifluoromethyl-1,3,4-thiadia zol-2-yl)oxy!acetamide 失效
标题翻译：制备N-（4-氟苯基）-N-（1-甲基乙基）-2 - [（5-三氟甲基-1,3,4-噻二唑-2-基）氧基]乙酰胺的方法
公开(公告)号：US5792872A
公开(公告)日：1998-08-11
申请号：US989564
申请日：1997-12-12
申请人： Vidyanatha A. Prasad , Jacqueline M. Applegate , Daniel M. Wasleski , Klaus Jelich
发明人： Vidyanatha A. Prasad , Jacqueline M. Applegate , Daniel M. Wasleski , Klaus Jelich
IPC分类号： A01N43/824 , C07D285/12 , C07D285/13
CPC分类号： C07D285/13
摘要： The present invention relates to a process for making N-(4-fluorophenyl)-N-(1-methylethyl)-2-�(5-(trifluoromethyl)-1,3,4-thiadiazol-2-yl)oxy!acetamide, which process includes the steps of reacting 2-(methylsulfonyl)-5-(trifluoromethyl)-1,3,4,-thiadiazole with N-(4-fluorophenyl)-2-hydroxy-N(1-methylethyl)acetamide in an aprotic, aromatic solvent with aqueous alkali to form an aqueous phase and an organic phase, separating the aqueous and organic phases and recovering the N-(4-fluorophenyl)-N-(1-methylethyl)-2-�(5-(trifluoromethyl)-1,3,4-thiadiazol-2-yl)oxy!acetamide from the organic phase. A preferred solvent and aqueous alkali are toluene and aqueous sodium hydroxide, respectively.
摘要翻译：本发明涉及制备N-（4-氟苯基）-N-（1-甲基乙基）-2 - [（5-（三氟甲基）-1,3,4-噻二唑-2-基）氧基]乙酰胺，该方法包括使2-（甲基磺酰基）-5-（三氟甲基）-1,3,4， - 噻二唑与N-（4-氟苯基）-2-羟基-N（1-甲基乙基）乙酰胺反应的步骤非质子芳族溶剂与水溶液形成水相和有机相，分离水相和有机相，并回收N-（4-氟苯基）-N-（1-甲基乙基）-2 - [（5-（三氟甲基））-1,3,4-噻二唑-2-基）氧基]乙酰胺。优选的溶剂和碱水溶液分别是甲苯和氢氧化钠水溶液。

9. 发明授权

US5856499A Synthesis of 2-(methysulfonyl)-5-(trifluoro-methyl)-,3,4-thiadiazole via oxidation of 2-(methylthio)-5-(trifluoromethyl)-1,3,4-thiadiazole with glacial acetic acid 失效
标题翻译：通过2-（甲硫基）-5-（三氟甲基）-1,3,4-噻二唑与冰醋酸的氧化合成2-（甲磺酰基）-5-（三氟甲基） - ，3,4-噻二唑
公开(公告)号：US5856499A
公开(公告)日：1999-01-05
申请号：US989594
申请日：1997-12-12
申请人： Vidyanatha A. Prasad , Jacqueline M. Applegate , Klaus Jelich , Achim Noack
发明人： Vidyanatha A. Prasad , Jacqueline M. Applegate , Klaus Jelich , Achim Noack
IPC分类号： B01J31/04 , C07B61/00 , C07D285/12 , C07D285/125
CPC分类号： C07D285/125
摘要： The present invention provides a process for making thiadiazole sulfones. The present process is used to make 2-(methylsulfonyl)-5-(trifluoromethyl)-1,3,4-thiadiazole. 2-(Methylsulfonyl)-5-(trifluoromethyl)-1,3,4-thiadiazole is made using catalytic oxidation in the presence of a suitable oxidizing agent. The catalyst used for the oxidation reaction is glacial acetic acid.
摘要翻译：本发明提供了制备噻二唑砜的方法。本方法用于制备2-（甲基磺酰基）-5-（三氟甲基）-1,3,4-噻二唑。在合适的氧化剂存在下，使用催化氧化制备2-（甲基磺酰基）-5-（三氟甲基）-1,3,4-噻二唑。用于氧化反应的催化剂是冰醋酸。

10. 发明授权

US06545172B1 Processes for the production of methyl dithiocarbazinate 有权
标题翻译：生产二硫代肼基甲酸甲酯的方法
公开(公告)号：US06545172B1
公开(公告)日：2003-04-08
申请号：US10124850
申请日：2002-04-18
申请人： Vidyanatha A. Prasad , Klaus Jelich , Dennis E. Jackman
发明人： Vidyanatha A. Prasad , Klaus Jelich , Dennis E. Jackman
IPC分类号： C07C33300
CPC分类号： C07C337/02
摘要： A process for the production of methyl dithiocarbazinate includes the steps of providing a mixture comprising hydrazine, solvent, carbon disulfide and base; adding methyl bromide to the mixture; cooling the reaction mixture; and recovering methyl dithiocarbazinate. The methyl dithiocarbazinate may be recovered by filtering the reaction mixture to yield a solid methyl dithiocarbazinate retentate and a liquid filtrate; acidifying the filterate with a mineral acid; and adding methyl isobutylketone to the acidified filterate.
摘要翻译：制备二硫代肼基甲酸甲酯的方法包括提供包含肼，溶剂，二硫化碳和碱的混合物的步骤; 向混合物中加入甲基溴; 冷却反应混合物; 并回收二硫代肼基甲酸甲酯。可以通过过滤反应混合物回收二硫代肼基甲酸甲酯，得到二硫代肼基甲酸固体甲基季戊四醇酯和液体滤液; 用无机酸酸化过滤物; 并向酸化的过滤器中加入甲基异丁基酮。

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