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1. 发明授权

US4246196A Diaminophenyl ureas 失效
标题翻译：二氨基苯脲
公开(公告)号：US4246196A
公开(公告)日：1981-01-20
申请号：US105500
申请日：1979-12-20
申请人： Otto Arndt , Theodor Papenfuhs , Peter Bohme , Wolfgang Tronich , Bernhard Mees
发明人： Otto Arndt , Theodor Papenfuhs , Peter Bohme , Wolfgang Tronich , Bernhard Mees
IPC分类号： C07B61/00 , C07C67/00 , C07C239/00 , C07C275/40 , C07D235/02 , C07D235/26 , C07C127/19
CPC分类号： C07C275/40 , C07D235/26
摘要： Diaminophenyl ureas of the formula ##STR1## in which R is an inert substituent, are obtained from the corresponding dinitrophenyl urea by way of reduction, especially catalytic hydrogenation. Through a cyclization process, while splitting off ammonia, these ureas yield the corresponding aminobenzimidazolones, advantageously without an intermediate isolation of the diaminophenyl ureas.
摘要翻译：其中R为惰性取代基的式“IMAGE”的二氨基苯脲通过还原，特别是催化氢化由相应的二硝基苯脲获得。通过环化过程，在分解氨时，这些脲产生相应的氨基苯并咪唑酮，有利地不用二氨基苯脲的中间分离。

2. 发明授权

US4552970A Solvated salts of dinitrophenylcyanamides, and a process for the preparation thereof 失效
标题翻译：二硝基苯基氰胺的溶剂化盐及其制备方法
公开(公告)号：US4552970A
公开(公告)日：1985-11-12
申请号：US576168
申请日：1984-02-01
申请人： Otto Arndt , Theodor Papenfuhs , Wolfgang Tronich
发明人： Otto Arndt , Theodor Papenfuhs , Wolfgang Tronich
IPC分类号： C07C261/04 , C07C261/00 , C07C273/06 , C07C275/30 , C07C125/08 , C07C127/19
CPC分类号： C07C275/30
摘要： Compounds of the formula I ##STR1## in which X denotes hydrogen, fluorine, chlorine or bromine, Y and Z denote hydrogen, lower alkyl or lower alkoxy, M denotes sodium, potassium or one equivalent of calcium and L denotes a dipolar aprotic solvent, are obtained from compounds of the formula II ##STR2## in which X, Y and Z have the abovementioned meanings, and a metal cyanamide of the formula IIIM.sub.2 N--CNin which M has the abovementioned meaning, in a dipolar aprotic solvent, which after the reaction is substantially removed, whereupon a lower molecular weight aliphatic alcohol is added to the residue and the product precipitated is isolated. Nitrophenylureas of the formula IV ##STR3## in which X, Y and Z have the abovementioned meanings, are obtained from the compounds of the formula I by acid hydrolysis.
摘要翻译：其中X表示氢，氟，氯或溴的式I“IMA”的化合物，Y和Z表示氢，低级烷基或低级烷氧基，M表示钠，钾或1当量的钙，L表示偶极非质子溶剂，由其中X，Y和Z具有上述含义的式II“IMAGE”的化合物和其中M具有上述含义的式IIIM2N-CN的金属氨基氰在偶极非质子传递溶剂中得到，后者为基本上除去反应物，然后向残余物中加入较低分子量的脂族醇，分离析出的产物。其中X，Y和Z具有上述含义的式IV“IMAGE”的硝基苯基脲通过酸水解得自式I化合物。

3. 发明授权

US4908478A Single-vessel process for preparing 2-acetaminonaphthalene-6-sulfonic acid of high purity 失效
标题翻译：用于制备高纯度2-乙酰氨基萘-6-磺酸的单容器方法
公开(公告)号：US4908478A
公开(公告)日：1990-03-13
申请号：US271376
申请日：1988-11-10
申请人： Otto Arndt , Theodor Papenfuhs
发明人： Otto Arndt , Theodor Papenfuhs
IPC分类号： B01J27/00 , C07C67/00 , C07C301/00 , C07C303/06 , C07C303/22 , C07C309/51
CPC分类号： C07C309/51
摘要： A single-vessel process for preparing 2-acetaminonaphthalene-6-sulfonic acid of high purity by sulfonating 2-hydroxynaphthalene with concentrated sulfuric acid, converting the 2-hydroxynaphthalenesulfonic acid formed with ammonia in the presence of ammonium hydrogensulfite into 2-amino-naphthalene-6-sulfonic acid (Bucherer reaction) and N-acetylating the latter to give 2-acetaminonaphthalene-6-sulfonic acid, which comprises, after diluting the sulfonating melt with water, substantially removing any impurities still present in the resulting aqueous solution of 2-hydroxynaphthalene-6-sulfonic acid, in particular 2-hydroxynaphthalene, by extraction with toluene or xylene and/or clarification using active carbon.
摘要翻译：通过用浓硫酸磺化2-羟基萘来制备高纯度2-乙酰氨基萘-6-磺酸的单容器方法，将在亚硫酸氢铵存在下由氨形成的2-羟基萘磺酸转化为2-氨基 - 萘 - 6-磺酸（Bucherer反应）和N-乙酰化后，得到2-乙酰氨基萘-6-磺酸，其包括在用水稀释磺化熔体之后，基本上除去所得到的2- 羟基萘-6-磺酸，特别是2-羟基萘，通过用甲苯或二甲苯萃取和/或使用活性炭澄清。

4. 发明授权

US5151532A Process for the production of high-purity tetrachloro-1,4-benzoquinone 失效
标题翻译：生产高纯度四氯丙烯-1,4-苯并噻唑酮的方法
公开(公告)号：US5151532A
公开(公告)日：1992-09-29
申请号：US724499
申请日：1991-06-27
申请人： Otto Arndt , Theodor Papenfuhs
发明人： Otto Arndt , Theodor Papenfuhs
IPC分类号： C07C50/24 , C07C37/62 , C07C45/00 , C07C46/00 , C07C46/06 , C07C67/00
CPC分类号： C07C46/00 , C07C37/62 , C07C46/06
摘要： A process for the preparation of high-purity tetrachloro-1,4-benzoquinone by the action of hydrogen peroxide and hydrochloric acid on hydroquinone, which comprises causing 3.8 top 4.2 times the molar quantity of 30 to 37% hydrochloric acid and 1.9 to 2.1 times the molar quantity of 50 to 35% hydrogen peroxide, to act at 5 to 50.degree. C. on 1 mole of hydroquinone in at least 12 times the molar quantity of 30 to 37% hydrochloric acid, then heating the resulting suspension, which essentially contains 2,5-dichlorohydroquinone, to 45 to 55.degree. C. and again causing to act on it, at 50 to 95.degree. C., 3.8 to 4.2 times the molar quantity of 30 to 37% hydrochloric acid and 1.9 to 2.1 times the molar quantity of 50 to 35% hydrogen peroxide, in each case based on the hydroquinone used, and finally adding to the suspension, which is now essentially composed of trichloro-1,4-benzoquinone, 1.9 to 2.1 times the molar quantity of hydrochloric acid of the said concentration range, and 0.95 to 1.05 times the molar quantity of hydrogen peroxide of the said concentration range, in each case based on the hydroquinone used, at 95 to 115.degree. C., sufficiently slowly for no chlorine to escape.
摘要翻译：一种通过过氧化氢和盐酸对氢醌的作用制备高纯度四氯-1,4-苯醌的方法，其包括使3.8倍上升4.2倍摩尔量的30至37％盐酸和1.9至2.1倍摩尔量为50至35％的过氧化氢，以5至50℃在1摩尔氢醌中至少12倍摩尔量的30至37％盐酸作用，然后加热得到的悬浮液，其基本上含有 2,5-二氯对苯二酚，至45至55℃，并再次引起其作用，在50至95℃，摩尔量为30至37％盐酸的3.8至4.2倍，摩尔数的1.9至2.1倍数量为50〜35％的过氧化氢，在各种情况下都是以所使用的氢醌为基准，最后加入到现在基本上由三氯-1,4-苯醌组成的悬浮液中，盐酸的摩尔量为1.9〜2.1倍该浓度范围为0.95〜1.05倍所述浓度范围内的摩尔量的过氧化氢，在每种情况下，基于所使用的氢醌，在95至115℃下，足够缓慢地没有氯逸出。

5. 发明授权

US5149850A Process for the production of high-purity tetrachloro-1,4-benzoquinone 失效
标题翻译：生产高纯度四氯丙烯-1,4-苯并噻唑酮的方法
公开(公告)号：US5149850A
公开(公告)日：1992-09-22
申请号：US726625
申请日：1991-06-28
申请人： Otto Arndt , Theodor Papenfuhs
发明人： Otto Arndt , Theodor Papenfuhs
IPC分类号： C07C37/62 , C07C45/00 , C07C46/00 , C07C46/06 , C07C50/24 , C07C67/00
CPC分类号： C07C46/00 , C07C37/62 , C07C46/06
摘要： A process for the production of high-purity tetrachloro-1,4-benzoquinone by the action of chlorine and hydrochloric acid on hydroquinone which comprises causing 1.9 to 2.1 times the molar quantity of gaseous chlorine to act at temperatures from 5.degree. to 15.degree. C. on 1 mol of hydroquinone in 6 to 7 times the molar quantity of 30 to 37% hydrochloric acid, then diluting the resulting suspension, essentially containing 2,5-dichlorohydroquinone, with 2 to 3 parts of water, relative to hydroquinone employed, and initially warming to a temperature from 20.degree. to 30.degree. C., subsequently introducing 1.9 to 2.1 times the molar quantity of chlorine gas in an air atmosphere while raising the temperature to 90.degree.-100.degree. C. with simultaneous dilution with 3.5 to 4.5 parts of water, relative to hydroquinone employed, and finally introducing 1 to 2 times the molar quantity of gaseous chlorine, relative to hydroquinone employed, at temperatures from 100.degree. to 115.degree. C.
摘要翻译：通过氯和盐酸对氢醌的作用生产高纯度四氯-1,4-苯醌的方法，其包括使气态氯的摩尔量的1.9至2.1倍在5至15℃的温度下起作用在1摩尔氢醌中的摩尔量为30至37％盐酸的6至7倍，然后相对于所用氢醌将所得悬浮液（基本上含有2,5-二氯对苯二酚）稀释至2至3份水，和最初升温至20℃至30℃，随后将空气气氛中的氯气的摩尔量引入1.9至2.1倍，同时将温度升至90℃-100℃，同时用3.5至4.5份稀释的水，相对于所使用的氢醌，并且最终在100-115℃的温度下，相对于所用的氢醌，引入1至2倍的气态氯的摩尔量。

6. 发明授权

US4613698A Process for the preparation of 6-chloro-2,4-dinitroaniline 失效
标题翻译：制备6-氯-2,4-二硝基苯胺的方法
公开(公告)号：US4613698A
公开(公告)日：1986-09-23
申请号：US706050
申请日：1985-02-27
申请人： Otto Arndt , Theodor Papenfuhs
发明人： Otto Arndt , Theodor Papenfuhs
IPC分类号： C07C209/74 , C07C67/00 , C07C209/00 , C07C211/52 , C07C85/24
CPC分类号： C07C209/74
摘要： Process for the preparation of 6-chloro-2,4-dinitroaniline by chlorination of 2,4-dinitroaniline with sodium hypochlorite in water using acid, which comprises carrying out the chlorination in the presence of a mineral acid or strong organic acid at a pH value .ltoreq.0 and in the presence of a dispersing agent at temperatures of about 40.degree. to 50.degree. C. and, when the chlorination has ended, either (a) filtering the resulting acid aqueous dispersion hot and washing the filtered reaction product with hot aqueous alkali solution, or (b) initially rendering the resulting acid aqueous dispersion alkaline with aqueous alkali solution and then filtering the mixture hot and subsequently washing the filtered reaction product with hot dilute mineral acid.
摘要翻译：通过使用酸在水中使用次氯酸钠氯化2,4-二硝基苯胺来制备6-氯-2,4-二硝基苯胺的方法，其包括在无机酸或强有机酸的存在下在pH下进行氯化在分散剂存在下，在约40℃至50℃的温度下，并且当氯化结束时，（a）将所得的酸水分散体过滤，并将过滤的反应产物用热碱水溶液，或（b）最初将所得酸水性分散体用碱性水溶液碱化，然后热过滤混合物，随后用热稀无机酸洗涤过滤的反应产物。

7. 发明授权

US4540832A Process for the preparation of 6-chloro-2,4-dinitrophenol 失效
标题翻译： 6-氯-2,4-二硝基苯酚的制备方法
公开(公告)号：US4540832A
公开(公告)日：1985-09-10
申请号：US604072
申请日：1984-04-26
申请人： Otto Arndt , Theodor Papenfuhs
发明人： Otto Arndt , Theodor Papenfuhs
IPC分类号： C07C67/00 , C07C201/00 , C07C201/12 , C07C205/26 , C07C79/28 , C07C79/32
CPC分类号： C07C201/12
摘要： A process for the preparation of 6-chloro-2,4-dinitrophenol in a high yield and in a high degree of purity by saponifying 2,4-dinitrochlorobenzene and/or 2,4-dinitrophenyl alkyl ethers of the formula ##STR1## in which m denotes the number 2, 3 or 4 and n denotes the number 1 or 2, by means of aqueous sodium hydroxide or potassium hydroxide solution and chlorinating the resulting 2,4-dinitrophenol with sodium hypochlorite, which comprises chlorinating the 2,4-dinitrophenol, without prior isolation as an intermediate, in aqueous suspension at a pH value of 3.5-7 by means of chlorine bleach liquor at temperatures of 5.degree. to 20.degree. C.
摘要翻译：通过将式“IMAGE”的2,4-二硝基氯苯和/或2,4-二硝基苯基烷基醚皂化，以高产率和高纯度制备6-氯-2,4-二硝基苯酚的方法其中m表示数字2,3或4，n表示数字1或2，用氢氧化钠水溶液或氢氧化钾溶液洗涤，并用次氯酸钠氯化所得的2,4-二硝基苯酚，其包括将2,4- 二硝基酚在没有预先分离为中间体的情况下，在pH值为3.5-7的水悬浮液中，通过氯漂白液在5至20℃的温度下进行。

8. 发明授权

US4487725A Process for the preparation of N-acetylaminoarylsulfonic acids in sulfuric acid as solvent 失效
标题翻译：在硫酸中作为溶剂制备N-乙酰氨基芳基磺酸的方法
公开(公告)号：US4487725A
公开(公告)日：1984-12-11
申请号：US495510
申请日：1983-05-17
申请人： Otto Arndt , Theodor Papenfuhs
发明人： Otto Arndt , Theodor Papenfuhs
IPC分类号： C07C303/04 , C07C67/00 , C07C301/00 , C07C303/12 , C07C303/22 , C07C309/51 , C07C309/88 , C07C143/58 , C07C143/60
CPC分类号： C07C303/22
摘要： The invention relates to salt-free N-acetylaminoarylsulfonic acids, their preparation by acetylation with acetic anhydride or acetyl chloride, sulfuric acid, which can also contain a small amount of water and/or dimethylformamide and/or N-methylpyrrolidone, serving as the solvent, and the use of the N-acetylaminoarylsulfonic acids for the preparation of their acid chlorides.
摘要翻译：本发明涉及无盐N-乙酰氨基芳基磺酸，其通过用乙酸酐或乙酰氯乙酰化制备硫酸，其还可以含有少量作为溶剂的水和/或二甲基甲酰胺和/或N-甲基吡咯烷酮，以及使用N-乙酰氨基芳基磺酸制备其酰氯。

9. 发明授权

US4824962A Process for the preparation of naphthostyril 失效
标题翻译：制备萘普生的方法
公开(公告)号：US4824962A
公开(公告)日：1989-04-25
申请号：US170065
申请日：1988-03-14
申请人： Otto Arndt , Theodor Papenfuhs
发明人： Otto Arndt , Theodor Papenfuhs
IPC分类号： C07D209/92
CPC分类号： C07D209/92
摘要： Process for the preparation of naphthostyril by dissolving 1,8-naphthalimide in an aqueous solution of lithium hydroxide and potassium hydroxide while heating at 40.degree. C. to 80.degree. C., cooling the solution obtained to 14.degree. C. and seeding it at said temperature with a maximum of 1 mol-% of sodium 1,8-naphthalimide per 1 mol of 1,8-naphthalimide used, then adding chlorine bleaching liquor at 10.degree. C. to 20.degree. C., reductively removing excess active chlorine after the reaction has taken place, adjusting the alkaline aqueous solution produced of the alkali-metal salt of the 1-aminonaphthal-ene-8-carboxylic acid formed to a pH of 2.0 by adding acid and isolating the naphthostyril which precipitates in this process.
摘要翻译：通过在40℃至80℃下加热将1,8-萘二甲酰亚胺溶解在氢氧化锂和氢氧化钾的水溶液中而制备萘未斯特林的方法，将所得溶液冷却至14℃，并将其在所述温度，每1摩尔1,8-萘二甲酰亚胺使用1,8-萘二甲酰亚胺钠最多1摩尔％，然后在10℃至20℃下加入氯漂白液，然后还原除去过量的活性氯发生反应，通过加入酸调节形成pH为2.0的1-氨基萘-8-羧酸的碱金属盐产生的碱性水溶液，并分离出在该过程中析出的萘并三唑。

10. 发明授权

US4605767A Process for the preparation of 2,6-dichloro-4-nitroaniline 失效
标题翻译： 2,6-二氯-4-硝基苯胺的制备方法
公开(公告)号：US4605767A
公开(公告)日：1986-08-12
申请号：US734972
申请日：1985-05-16
申请人： Otto Arndt , Theodor Papenfuhs
发明人： Otto Arndt , Theodor Papenfuhs
IPC分类号： C07C209/74 , C07C67/00 , C07C209/00 , C07C211/52 , C07C85/24 , C07C87/60
CPC分类号： C07C209/74
摘要： Process for the preparation of 2,6-dichloro-4-nitroaniline by chlorination of 4-nitroaniline with chlorine bleaching liquor in water using acids, which comprises chlorinating 1 mole of 4-nitroaniline in 3-6 moles of hydrochloric acid (HCl) or nitric acid (HNO.sub.3) in the form of a dilute, aqueous acid in the presence of a dispersing agent which is stable under the reaction conditions, the chlorination initially being carried out at 5.degree. to 10.degree. C. and then at 15.degree.-20.degree. C. and, finally, after 90-95% of the 2-chloro-4-nitroaniline intermediately formed has been converted into 2,6-dichloro-4-nitroaniline, the temperature of the aqueous suspension being increased from 15.degree.-20.degree. C. to 70.degree. C., without further addition of chlorine bleaching liquor, and then by post-chlorinating, by renewed addition of chlorine bleaching liquor, at temperatures between 20.degree. and 70.degree. C., bringing the pH of the aqueous suspension to 9.0 and filtering off the 2,6-dichloro-4-nitroaniline formed and washing it with dilute mineral acid.
摘要翻译：通过使用酸在氯水中用氯漂白液氯化4-硝基苯胺的方法制备2,6-二氯-4-硝基苯胺的方法，该方法包括将1-6摩尔盐酸（HCl）中的1摩尔4-硝基苯胺氯化，或硝酸（HNO 3）为稀酸水溶液，在分散剂存在下，在反应条件下稳定，氯化最初在5〜10℃进行，然后在15〜-20℃ ℃，最后，90-95％的中间形成的2-氯-4-硝基苯胺已经转化为2,6-二氯-4-硝基苯胺，水悬浮液的温度从15°-20 在不进一步加入氯漂白液的情况下，通过后续氯化，通过在20℃至70℃的温度下再次加入氯漂白液，使水悬浮液的pH值达到70℃ 至9.0，滤出2,6-二氯-4-硝基苯胺 d用稀释的无机酸洗涤。

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