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1. 发明授权

US4599455A Process of purifying fluorinated carbonyl compound mixed with hydrogen fluoride 失效
标题翻译：纯化氟化羰基化合物与氟化氢混合的方法
公开(公告)号：US4599455A
公开(公告)日：1986-07-08
申请号：US604534
申请日：1984-04-27
申请人： Yutaka Maruyama , Junji Negishi , Katuyoshi Murata , Yutaka Katsuhara
发明人： Yutaka Maruyama , Junji Negishi , Katuyoshi Murata , Yutaka Katsuhara
IPC分类号： C07C47/14 , C07C45/00 , C07C45/78 , C07C45/85 , C07C49/16 , C07C49/167 , C07C67/00 , B01D53/14
CPC分类号： C07C45/783 , C07C45/85
摘要： A fluorinated carbonyl compound ##STR1## where x is 2 or 3 and A represents CF.sub.3 or H, coexisting with hydrogen fluoride in a mixed gas is purified by first adjusting the temperature of the mixed gas to 100.degree.-300.degree. C. to cause decomposition of a usually coexisting complex of the fluorinated compound with HF and then bringing the hot mixed gas into contact with concentrated sulfuric acid maintained at 10.degree.-40.degree. C. Almost the entire amount of HF is absorbed in sulfuric acid and subsequently recovered, while the purified compound neither dissolves in sulfuric acid nor reacts with HF present in sulfuric acid.
摘要翻译：通过首先将混合气体的温度调节至100-300℃，将混合气体中与氟化氢共存的x为2或3，A表示CF 3或H的氟化羰基化合物＆lt; IMAGE＆gt; 的氟化合物与HF的通常共存的复合物，然后使热混合气体与保持在10 -40℃的浓硫酸接触。几乎全部量的HF被吸收在硫酸中并随后回收，而纯化的化合物既不溶于硫酸也不与存在于硫酸中的HF反应。

2. 发明授权

US4386223A Method of purifying hexafluoroacetone containing chlorofluoroacetones 失效
标题翻译：净化含氟氯丙酮六氟丙酮的方法
公开(公告)号：US4386223A
公开(公告)日：1983-05-31
申请号：US320079
申请日：1981-11-10
申请人： Toshikazu Kawai , Yutaka Maruyama , Junji Negishi , Akira Negishi
发明人： Toshikazu Kawai , Yutaka Maruyama , Junji Negishi , Akira Negishi
IPC分类号： C07C49/167 , C07C45/00 , C07C45/78 , C07C45/85 , C07C67/00
CPC分类号： C07C45/783 , C07C45/78 , C07C45/85
摘要： Crude hexafluoroacetone (HFA) containing chlorofluoroacetone(s) (CFA) as well as hydrogen halide(s) is purified by initially allowing the crude HFA to be absorbed in water to give an aqueous solution in which HFA and CFA are in the form of their respective hydrates, adding a calcium compound such as carbonate, hydroxide or oxide to the solution to neutralize the hydrogen halide(s), and decomposing the hydrated CFA by first adding an alkali metal compound such as K.sub.2 CO.sub.3 or Na.sub.2 CO.sub.3 or an alkaline earth metal compound such as Ca(OH).sub.2, Ba(OH).sub.2, CaO or BaO to the solution and subsequently adding a mineral acid such as HCl or H.sub.2 SO.sub.4 to the same solution. This procedure results in complete decomposition of CFA without causing decomposition of HFA and spontaneous separation of the liquid reaction system into two layers, one of which is exclusively HFA hydrate. Accordingly it is easy to separate pure HFA hydrate from the decomposed impurities.
摘要翻译：通过首先使粗HFA被吸收在水中来纯化含有氯氟丙酮（CFA）和卤化氢的粗六氟丙酮（HFA），其中HFA和CFA为其HFA和CFA形式的水溶液各自的水合物，向溶液中加入钙化合物如碳酸盐，氢氧化物或氧化物以中和卤化氢，并且通过首先加入碱金属化合物如K 2 CO 3或Na 2 CO 3或碱土金属化合物来分解水合CFA，作为Ca（OH）2，Ba（OH）2，CaO或BaO，然后向同一溶液中加入无机酸如HCl或H 2 SO 4。该过程导致CFA完全分解而不引起HFA分解，并将液体反应体系自发分离成两层，其中之一仅为HFA水合物。因此，容易将纯HFA水合物与分解的杂质分离。

3. 发明授权

US5017730A Process of preparing bis (trifluoromethylphenyl) methanol 失效
标题翻译：制备双（三氟甲基苯基）甲醇的方法
公开(公告)号：US5017730A
公开(公告)日：1991-05-21
申请号：US491969
申请日：1990-03-12
申请人： Yoshihiko Gotoh , Toshikazu Kawai , Junji Negishi
发明人： Yoshihiko Gotoh , Toshikazu Kawai , Junji Negishi
IPC分类号： C07C29/143 , C07C33/46 , C07C45/46 , C07C45/63 , C07C45/68 , C07C49/784 , C07C49/813
CPC分类号： C07C49/813 , C07C33/46 , C07C45/46 , C07C45/63 , C07C49/784
摘要： The invention provides a process for easily, efficiently and economically preparing bis(trifluoromethylphenyl)methanol from either toluoyl chloride or a trihalomethylbenzoyl chloride. First the starting compound is reacted with toluene in the presence of a strong acid catalyst such as a perfluoroalkylsulfonic acid to form a benzophenone derivative, CX.sub.3 C.sub.6 H.sub.4 --CO--C.sub.6 H.sub.4 CH.sub.3, wherein X is H, F, Cl or Br. Next, by chlorination the benzophenone derivative is converted into CY.sub.3 C.sub.6 H.sub.4 --CO--C.sub.6 H.sub.4 CCL.sub.3, wherein Y is F or Cl, and then the chlorinated intermediate is fluorinated into bis(trifluoromethyl)benzophenone. By reduction of carbonyl group of this benzophenone derivative the aimed compound is obtained.
摘要翻译：本发明提供了一种从甲苯酰氯或三卤代甲基苯甲酰氯容易，有效和经济地制备双（三氟甲基苯基）甲醇的方法。首先，在强酸催化剂例如全氟烷基磺酸的存在下，使起始化合物与甲苯反应形成二苯甲酮衍生物CX3C6H4-CO-C6H4CH3，其中X为H，F，Cl或Br。接下来，通过氯化，将二苯甲酮衍生物转化成CY3C6H4-CO-C6H4CCL3，其中Y是F或Cl，然后氯化的中间体被氟化成双（三氟甲基）二苯甲酮。通过还原该二苯甲酮衍生物的羰基，得到目标化合物。

4. 发明授权

US07199262B2 3-Hydroxypropyl ester of 2-trifluoromethylacrylic acid and process for producing same 有权
标题翻译： 2-三氟甲基丙烯酸3-羟丙酯及其制备方法
公开(公告)号：US07199262B2
公开(公告)日：2007-04-03
申请号：US11152144
申请日：2005-06-15
申请人： Takahisa Tada , Seiji Murata , Akihiro Fukui , Junji Negishi
发明人： Takahisa Tada , Seiji Murata , Akihiro Fukui , Junji Negishi
IPC分类号： C07C69/52 , C07C69/34 , C07C69/63
CPC分类号： C07C69/653
摘要： The invention relates to a novel compound, 3-hydroxypropyl ester of 2-trifluoromethyl acrylic acid, represented by the formula [1]. The invention further relates to a process for producing the compound. This process includes reacting 2-trifluoromethylacrylic halide represented by the formula [2], wherein the halogen atom is F or Cl, with 1,3-propanediol represented by the formula [3], in the presence of a base
摘要翻译：本发明涉及由式[1]表示的2-三氟甲基丙烯酸的新型化合物3-羟丙基酯。本发明还涉及一种生产该化合物的方法。该方法包括使由式[2]表示的2-三氟甲基丙烯酰卤与式[3]表示的1,3-丙二醇反应，其中卤素原子为F或Cl，在碱的存在下

5. 发明授权

US4849557A Preparation of trifluoromethyltoluene from halomethylbenzotrifluoride 失效
标题翻译：由卤代甲基三氟甲苯制备三氟甲基甲苯
公开(公告)号：US4849557A
公开(公告)日：1989-07-18
申请号：US193061
申请日：1988-05-12
申请人： Takeshi Kondo , Junji Negishi , Yoshihiko Goto , Matsue Minezaki , Toshikazu Kawai
发明人： Takeshi Kondo , Junji Negishi , Yoshihiko Goto , Matsue Minezaki , Toshikazu Kawai
IPC分类号： C07C17/23 , C07C17/38 , C07C22/08
CPC分类号： C07C22/08 , C07C17/23 , C07C17/38
摘要： Trifluoromethyltoluene is obtained from a halomethylbenzotrifluoride, which is a relatively inexpensive material, by hydrogenating the halomethyl group of the starting compound to methyl group with hydrogen gas in the presence of a hydrogenation catalyst and an acid acceptor. Suitable examples of the halomethyl group to be hydrogenated are --CH.sub.2 Cl, --CH.sub.2 F, --CHClF, --CClF.sub.2 and --CF.sub.3. When the starting compound is bis(trifluromethyl)benzene, addition of either an alcohol or an alkali metal fluoride to the reaction system is effective for suppression of formation of xylene as a by-product, and xylene still contained in the reaction product can completely be removed by treatment with a sulfonating agent such as fuming sulfuric acid.
摘要翻译：通过在氢化催化剂和酸受体的存在下，用氢气将起始化合物的卤代甲基氢化成甲基，由相对便宜的卤代甲基三氟甲苯得到三氟甲基甲苯。待氢化的卤代甲基的合适实例是-CH 2 Cl，-CH 2 F，-CHClF，-CClF 2和-CF 3。当起始化合物为双（三氟甲基）苯时，向反应体系中加入醇或碱金属氟化物对于抑制作为副产物形成二甲苯是有效的，反应产物中仍含有的二甲苯可以完全通过用磺化剂如发烟硫酸处理除去。

6. 发明授权

US07002043B2 Process for producing 1,1,1-trifluoroacetone 失效
标题翻译：制备1,1,1-三氟丙酮的方法
公开(公告)号：US07002043B2
公开(公告)日：2006-02-21
申请号：US10448318
申请日：2003-05-30
申请人： Masanori Tsukamoto , Fumiyoshi Yoshikawa , Masataka Fujimoto , Naoto Takada , Yoshikazu Sugimori , Junji Negishi
发明人： Masanori Tsukamoto , Fumiyoshi Yoshikawa , Masataka Fujimoto , Naoto Takada , Yoshikazu Sugimori , Junji Negishi
IPC分类号： C07C45/65
CPC分类号： C07C49/167 , C07C45/65
摘要： The invention relates to a process for producing 1,1,1-trifluoroacetone, which is useful as an intermediate of pharmaceuticals and agricultural chemicals, or as a reagent for introducing fluorine-containing groups. This process includes the step of conducting a hydrogenolysis of a halogenated trifluoroacetone, which is represented by the formula [1], by a hydrogen gas, in a liquid phase containing water, in the presence of a catalyst containing a transition metal, where X represents a chlorine, bromine or iodine, and n represents an integer from 1 to 3. It is possible by the process to easily produce 1,1,1-trifluoroacetone with high purity.
摘要翻译：本发明涉及一种生产1,1,1-三氟丙酮的方法，其可用作药物和农药的中间体，或用作引入含氟基团的试剂。该方法包括在含有过渡金属的催化剂的存在下，通过氢气在含有水的液相中，通过式[1]表示的卤代三氟丙酮的氢解，步骤 =“CHEM-US-00001”num =“000

7. 发明授权

US06774266B2 Process for producing 1,1,1-trifluoroacetone 失效
标题翻译：制备1,1,1-三氟丙酮的方法
公开(公告)号：US06774266B2
公开(公告)日：2004-08-10
申请号：US10299996
申请日：2002-11-20
申请人： Masanori Tsukamoto , Takashi Sakaya , Takayuki Nishimiya , Junji Negishi
发明人： Masanori Tsukamoto , Takashi Sakaya , Takayuki Nishimiya , Junji Negishi
IPC分类号： C07C4500
CPC分类号： C07C45/65 , C07C49/167
摘要： A process for producing 1,1,1-trifluoroacetone includes the step of conducting in a gas phase a hydrogenolysis of a tetrafluoroacetone, which is represented by the general formula [1], by a hydrogen gas in the presence of a catalyst containing a transition metal, where X represents a chlorine, bromine or iodine, and n represents an integer from 0 to 2.
摘要翻译：制备1,1,1-三氟丙酮的方法包括在含有过渡金属催化剂的催化剂存在下，在气相中进行由通式[1]表示的四氟丙酮的氢解的工序，金属，其中X表示氯，溴或碘，n表示0至2的整数。

8. 发明申请

US20060009653A1 3-Hydroxypropyl ester of 2-trifluoromethylacrylic acid and process for producing same 有权
标题翻译： 2-三氟甲基丙烯酸3-羟丙酯及其制备方法
公开(公告)号：US20060009653A1
公开(公告)日：2006-01-12
申请号：US11152144
申请日：2005-06-15
申请人： Takahisa Tada , Seiji Murata , Akihiro Fukui , Junji Negishi
发明人： Takahisa Tada , Seiji Murata , Akihiro Fukui , Junji Negishi
IPC分类号： C07C69/653
CPC分类号： C07C69/653
摘要： The invention relates to a novel compound, 3-hydroxypropyl ester of 2-trifluoromethyl acrylic acid, represented by the formula [1]. The invention further relates to a process for producing the compound. This process includes reacting 2-trifluoromethylacrylic halide represented by the formula [2], wherein the halogen atom is F or Cl, with 1,3-propanediol represented by the formula [3], in the presence of a base.
摘要翻译：本发明涉及由式[1]表示的2-三氟甲基丙烯酸的新型化合物3-羟丙基酯。本发明还涉及一种生产该化合物的方法。该方法包括使由式[2]表示的2-三氟甲基丙烯酰卤反应，其中卤素原子为F或Cl，与由式[3]表示的1,3-丙二醇在碱存在下反应。

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