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1.发明授权
公开(公告)号：US4191711A
公开(公告)日：1980-03-04
申请号：US925494
申请日：1978-07-17
摘要： A process for the preparation of 3,4-dichlorobenzotrichloride, 3,4,5-trichlorobenzotrichloride, 2,4,5-trichlorobenzotrichloride or 2,3,4,5-tetrachlorobenzotrichloride which comprises contacting p-chlorobenzotrichloride of the formula ##STR1## with chlorine or an agent which releases chlorine at a temperature between 0.degree. C. and 180.degree. C. in the presence of an iron (III) chloride or aluminum chloride catalyst or a mixture of iron (III) chloride or aluminum chloride with sulfur dichloride or disulfur dichloride.
摘要翻译： 一种制备3,4-二氯一氯三苯，3,4,5-三氯三氯甲烷，2,4,5-三氯三氯甲烷或2,3,4,5-四氯一氯三氯化物的方法，其包括使式（IMAGE）的对氯三氯苯 I）与氯或在氯化铁（III）或氯化铝催化剂或氯化铁（III）或氯化铝的混合物存在下在0℃至180℃之间的温度释放氯的试剂与氯 二氯化硫或二氯化硫。
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2.发明授权
公开(公告)号：US4176133A
公开(公告)日：1979-11-27
申请号：US953048
申请日：1978-10-19
申请人： Manfred Lenthe , Gerhard Dankert
发明人： Manfred Lenthe , Gerhard Dankert
IPC分类号： C07C255/25 , C07C67/00 , C07C253/00 , C07C255/24 , C07C121/43
CPC分类号： C07C255/00
摘要： In the recovery of N,N-dimethylaminoacetonitrile from a mixture thereof with water by extraction with an organic solvent thereby to form an aqueous phase and an organic solvent phase containing the nitrile, separating the organic phase, and recovering the nitrile from the organic solvent, the improvement which comprises employing 1,2-dichlorobenzene as the organic solvent. Recovery of the nitrile from the organic solvent can be accomplished by distilling of the nitrile, the undistilled solvent being recycled for further use.
摘要翻译： 通过用有机溶剂萃取从其与水的混合物中回收N，N-二甲基氨基乙腈，从而形成含有腈的水相和有机溶剂相，分离有机相，并从有机溶剂中回收腈， 包括使用1,2-二氯苯作为有机溶剂的改进。 从有机溶剂中回收腈可以通过蒸馏腈来完成，未蒸馏的溶剂被再循环用于进一步的使用。
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公开(公告)号：US4486611A
公开(公告)日：1984-12-04
申请号：US412643
申请日：1982-08-30
摘要： A process for the isolation of a dihydroxybenzene-monoether from a reaction mixture containing solvent, ether and unreacted dihydroxybenzene, comprising contacting the reaction mixture with at least one hydrocarbon which is not miscible or only partially miscible with the reaction mixture, the ether selectively entering the hydrocarbon. Advantageously the reaction for the preparation of the monoether is carried out in an alcohol, a ketone, a dipolar aprotic solvent or a polyhydroxyalkyl ether, or a mixture thereof with water, the hydrocarbon used as extracting agent has a boiling point between about 80.degree. and 300.degree. C., and the extraction is carried out in the presence of water whereby there is an increase in the selectivity of the extraction.
摘要翻译： 一种从含有溶剂，醚和未反应的二羟基苯的反应混合物中分离二羟基苯 - 单醚的方法，包括使反应混合物与至少一种与反应混合物不混溶或仅部分混溶的烃接触，所述醚选择性地进入 烃。 有利地，用于制备单醚的反应在醇，酮，偶极非质子溶剂或多羟基烷基醚或其与水的混合物中进行，用作萃取剂的烃的沸点在约80℃和 300℃，萃取在水的存在下进行，由此萃取的选择性增加。
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公开(公告)号：US4321204A
公开(公告)日：1982-03-23
申请号：US170443
申请日：1980-07-21
CPC分类号： C07C43/23 , C07D307/86
摘要： In the preparation of a 7-hydroxycoumaran of the formula ##STR1## in which Z is a hydrogen atom or a substituent which is inert under the subsequent reaction conditions,R.sup.1 is a hydrogen atom or a C.sub.1 to C.sub.4 -alkyl radical, andn is 1, 2 or 3wherein a pyrocatechol of the formula ##STR2## is reacted with an allyl compound of the formula ##STR3## in which Y is a halogen atom, a C.sub.1 to C.sub.4 -alkyl-sulphonate radical or an aryl-sulphonate radical,to form the mono-ether of the pyrocatechol in a first stage, and in a second stage, of the pyrocatechol monoether formed in the first stage is rearranged to a 3-alkenylpyrocatechol, and in a third stage the 3-alkenylpyrocatechol formed in the second stage, is cyclized, the improvement which comprises stages. (b) carrying out the second stage at a pH of about 2-8. Advantageously glycol monomethyl ether is employed as the solvent in all stages and the third stage is carried out with a residence time of about 1-30 minutes and with a narrow residence time spectrum corresponding to a Bodenstein-index 5, optionally in the presence of an iron salt.
摘要翻译： 在制备其中Z为氢原子的式“IMAGE”的7-羟基香豆素或在随后的反应条件下为惰性的取代基时，R 1为氢原子或C 1至C 4 - 烷基，n为 1,2或3其中式IMAMA的邻苯二酚与其中Y是卤素原子，C1-C4烷基磺酸根基或芳基 - 磺酸根基团的式“IMAGE”的烯丙基化合物反应， 在第一阶段中形成邻苯二酚的单醚，在第二阶段将第一阶段中形成的邻苯二酚单醚重新排列为3-链烯基邻苯二酚，第三阶段中形成的3-链烯基邻苯二酚 阶段，循环，改进包括阶段。 （b）在约2-8的pH下进行第二阶段。 在所有阶段中，优选使用二醇单甲醚作为溶剂，第三阶段以约1-30分钟的停留时间和对应于博登斯坦指数5的窄停留时间光谱进行，任选地在 铁盐
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5.发明授权Process for the preparation of 2-(4-chlorophenylethyl)-2-tert.-butyl-oxirane 失效2-（4-氯苯乙基）-2-叔丁基 - 环氧乙烷的制备方法
公开(公告)号：US4988829A
公开(公告)日：1991-01-29
申请号：US373770
申请日：1989-06-30
申请人： Paul Fiedler , Martin Littmann , Manfred Lenthe , Achim Noak , Gerd Siekmann
发明人： Paul Fiedler , Martin Littmann , Manfred Lenthe , Achim Noak , Gerd Siekmann
IPC分类号： C07D303/08
CPC分类号： C07D303/08
摘要： A process for making the known fungicide intermediate 2-(4-chlorophenyl ethyl)-2-tert.-butyloxirane of the formula ##STR1## comprising (a) mixing a solution of trimethylsulphonium bromide of the formula(CH.sub.3).sub.3 S.sup..sym. Br.sup..crclbar. (II) in a methanol/toluene mixture with preheated toluene and simultaneously distilling off a methanol/toluene mixture at a temperature between 65.degree. and 110.degree. C. until a suspension having a solids content between 10 and 70% by weight is formed, and(b) reacting the suspension of trimethylsulphonium bromide in toluene thus obtained with 1-(4-chlorophenyl)-4,4-dimethylpentan-3-one of the formula ##STR2## in the presence of solid potassium hydroxide, diethylene glycol and water at a temperature between 20.degree. and 120.degree. C., the amounts of the reaction components being such that per mole of 1-(4-chlorophenyl)-4,4-dimethylpentan-3-one of the formula (III) there are presentbetween 1 and 2 moles of trimethylsulphonium bromide of the formula (II),between 2 and 3 moles of solid potassium hydroxide and alsobetween 0.1 and 10% by weight of diethylene glycol and between 0.5 and 12% by weight of water, relative to 1-(4-chlorophenyl)-4,4-dimethylpentan-3-one of the formula (III).
摘要翻译： 制备已知的杀真菌剂中间体式（I）的2-（4-氯苯基乙基）-2-叔丁基环氧乙烷的方法包括（a）将式（CH3）3S的三甲基锍溴化物 +）Br（ - ）（II）的甲醇/甲苯混合物中，同时在65-110℃的温度下蒸馏除去甲醇/甲苯混合物，直到固体含量为10至70％ ，并且（b）使由此获得的甲苯中的三甲基锍溴化物的悬浮液与式（III）的1-（4-氯苯基）-4,4-二甲基戊-3-酮在存在 固体氢氧化钾，二甘醇和水，温度在20℃至120℃之间，反应组分的量使得每摩尔1-（4-氯苯基）-4,4-二甲基戊-3-酮为 式（III）中存在1至2摩尔式（II）的三甲基锍溴化物，2至3小时 固体氢氧化钾和0.1至10重量％的二甘醇和0.5至12重量％的水相对于式（I）的1-（4-氯苯基）-4,4-二甲基戊-3-酮， （三）。
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6.发明授权
公开(公告)号：US4683308A
公开(公告)日：1987-07-28
申请号：US820510
申请日：1986-01-21
IPC分类号： B27K3/36 , C07D251/44 , C07F9/38 , C07F9/40 , C07F9/42 , D06M13/313
CPC分类号： C07F9/3826 , C07D251/44 , C07F9/4015 , C07F9/42 , D06M13/313
摘要： In the preparation of a 2-arylamino-4,6-dichloro-s-triazine of the formula ##STR1## in which R.sup.1 is an optionally substituted aryl radical, andR.sup.2 is hydrogen or alkyl,by reacting cyanuric chloride of the formula ##STR2## with a virtually water-insoluble arylamine of the formula ##STR3## at a temperature between 0.degree. and 100.degree. C., the improvement which comprises effecting the reaction in water at an acid pH in the presence of a virtually water-insoluble organic solvent. The resulting aqueous phase contains the triazine in such high purity and concentration that it can be used without further purification. The organic solvent can be recycled.
摘要翻译： 在制备式“IMAGE”的2-芳基氨基-4,6-二氯-s-三嗪的方法中，其中R 1是任选取代的芳基，R 2是氢或烷基，通过式 >在0℃至100℃的温度下具有式（IMAGE）的几乎不溶于水的芳基胺，其改进包括在几乎不溶于水的有机溶剂存在下，在酸性pH下进行水中的反应 。 所得水相含有如此高纯度和浓度的三嗪，其可以不经进一步纯化而使用。 有机溶剂可循环利用。
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公开(公告)号：US4647676A
公开(公告)日：1987-03-03
申请号：US612962
申请日：1984-05-23
IPC分类号： C07C41/16 , C07C41/38 , C07C43/23 , C07D307/86
摘要： A process for the isolation of a dihydroxybenzenemonoether from a reaction mixture containing solvent, ether and unreacted dihydroxybenzene, comprising contacting the reaction mixture with at least one hydrocarbon which is not miscible or only partially miscible with the reaction mixture, the ether selectively entering the hydrocarbon. Advantageously the reaction for the preparation of the monoether is carried out in an alcohol, a ketone, a dipolar aprotic solvent or a polyhydroxyalkyl ether, or a mixture thereof with water, the hydrocarbon used as extracting agent has a boiling point between about 80.degree. and 300.degree. C., and the extraction is carried out in the presence of water whereby there is an increase in the selectivity of the extraction.
摘要翻译： 一种从含有溶剂，醚和未反应的二羟基苯的反应混合物中分离出二羟基苯氰醚的方法，包括使反应混合物与至少一种与反应混合物不混溶或仅部分混溶的烃接触，醚选择性地进入烃。 有利地，用于制备单醚的反应在醇，酮，偶极非质子溶剂或多羟基烷基醚或其与水的混合物中进行，用作萃取剂的烃的沸点在约80℃和 300℃，萃取在水的存在下进行，由此萃取的选择性增加。
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公开(公告)号：US4383126A
公开(公告)日：1983-05-10
申请号：US315126
申请日：1981-10-26
申请人： Gerhard Buttner , Artur Judat , Udo Allenbach , Manfred Lenthe
发明人： Gerhard Buttner , Artur Judat , Udo Allenbach , Manfred Lenthe
CPC分类号： C07C41/16
摘要： A process for the preparation of a monoalkyl ether of a hydroxyphenol of the formula ##STR1## in which Z each independently is hydrogen or a substituent which is stable under the reaction conditions,R is lower alkyl, andn is 1, 2, 3 or 4,comprising reacting a hydroxyphenol of the formula ##STR2## with an alkyl halide, alkyl sulphonate or aryl sulphonate alkylating agent of the formulaR--Xin which X is a halogen atom, or an alkylsulphonyloxy or arylsulphonyloxy radical,at a temperature from about 130.degree. C. to 200.degree. C. and in the presence of an alkali metal base or alkaline earth metal base and of a diluent comprising a polyhydroxyalkyl ether having at least one OH group. Advantageously the base is sodium carbonate, sodium bicarbonate, potassium carbonate or potassium bicarbonate, the hydroxyphenol is pyrocatechol, the alkylating agent is isopropyl chloride, isopropyl C.sub.1-4 -alkyl-1-sulphonate, isopropyl benzenesulphonate or isopropyl tolyenesulphonate, and the polyhydroxyalkyl ether is glycol monomethyl ether, about 1.5 to 1.8 mols of alkylating agent and about 1 to 2 mols of the base being employed per mol of pyrocatechol, about 1.5 to 2.5 parts by weight of the glycol monomethyl ether being employed per part by weight of pyrocatechol, the reaction being effected in an inert atmosphere under elevated pressure.
摘要翻译： 制备式“IMAGE”的羟基苯酚的单烷基醚的方法，其中Z各自独立地为氢或在反应条件下稳定的取代基，R为低级烷基，n为1,2,3或 4，包括使式（ⅩⅧ）的羟基苯酚与其中X为卤素原子的式RX的烷基卤化物，烷基磺酸盐或芳基磺酸盐烷基化剂或烷基磺酰氧基或芳基磺酰氧基在约130℃ 在碱金属碱或碱土金属碱和包含具有至少一个OH基团的多羟基烷基醚的稀释剂的存在下进行。 有利地，碱是碳酸钠，碳酸氢钠，碳酸钾或碳酸氢钾，羟基苯酚是邻苯二酚，烷基化剂是异丙基氯，异丙基C 1-4 - 烷基-1-磺酸酯，异丙基苯磺酸酯或异丙基甲苯磺酸酯，多羟基烷基醚是 二醇单甲醚，约1.5-1.8摩尔烷基化剂和每摩尔邻苯二酚使用约1-2摩尔的碱，每重量份邻苯二酚使用约1.5-2.5重量份的二醇单甲醚， 反应在惰性气氛中在升高的压力下进行。
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公开(公告)号：US4360479A
公开(公告)日：1982-11-23
申请号：US276774
申请日：1981-06-24
申请人： Kurt Findeisen , Hans Kratzer , Manfred Lenthe
发明人： Kurt Findeisen , Hans Kratzer , Manfred Lenthe
IPC分类号： C07C255/17 , C07C51/08 , C07C67/00 , C07C253/00 , C07C255/40 , C07C255/56 , C07D253/06 , C07D253/07 , C07C51/083
CPC分类号： C07D253/07 , C07C255/00
摘要： This invention relates to a new process for the preparation of acyl cyanides of the general formulaR.sup.1 --CO--CN (I)wherein R.sup.1 is an optionally substituted alkyl radical up to 18 carbon atoms, an optionally substituted cycloalkyl radical with 3 to 12 carbon atoms, an optionally substituted aryl radical or an optionally substituted 5- or 6-membered heterocyclic radical, which can additionally also be fused with a benzene ring, which process comprises reacting a carboxylic acid anhydride of the formulaR.sup.1 --CO--O--CO--R.sup.1 (II)with an alpha-hydroxynitrile of the formula ##STR1## in which R.sup.2 and R.sup.3 are identical or different and represent a hydrogen atom, an optionally substituted alkyl radical with 1 to 18 carbon atoms, an optionally substituted cycloalkyl radical with 3 to 12 carbon atoms, an optionally substituted aryl radical or an optionally substituted 5- or 6-membered heterocyclic radical, which can additionally also be fused with a benzene ring. The acyl cyanides (I) are known compounds and can be used as starting material for the synthesis of herbicides.
摘要翻译： 本发明涉及用于制备通式为R 1 -CO-CN（I）的酰基氰的新方法，其中R 1为任选取代的至多18个碳原子的烷基，具有3至12个碳原子的任选取代的环烷基 ，任选取代的芳基或任选取代的5-或6-元杂环基，其还可以与苯环稠合，该方法包括使式R 1 -CO-O-CO-R 1的羧酸酐 （II）与式（III）的α-羟基腈，其中R 2和R 3相同或不同并且表示氢原子，任选取代的具有1至18个碳原子的烷基，任选取代的环烷基与 3至12个碳原子，任选取代的芳基或任选取代的5或6元杂环基，其还可以与苯环稠合。 酰基氰化物（I）是已知的化合物，可用作合成除草剂的原料。
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10.发明授权Preparation of chlorinated N-methyl-imidazoles and N-methyl-imidazolines 失效氯化N-甲基 - 咪唑和N-甲基 - 咪唑啉的制备
公开(公告)号：US4216332A
公开(公告)日：1980-08-05
申请号：US974411
申请日：1978-12-29
申请人： Manfred Lenthe , Gerhard Dankert
发明人： Manfred Lenthe , Gerhard Dankert
IPC分类号： C07C67/00 , C07C239/00 , C07C241/00 , C07C271/00 , C07D233/28 , C07D233/68
CPC分类号： C07D233/28 , C07D233/68
摘要： In the preparation of chlorinated N-methyl-imidazoles and N-methyl-imidazolines of the formula ##STR1## in which n represents the number 0, 1, 2 or 3 andm represents the number 0 or 1, a double bond being present between the C atoms in the 4-position and 5-position when m is 0, and a single bond being present when m is 1,by chlorinating N,N-dimethylaminoacetonitrile of the formula(CH.sub.3).sub.2 N--CH.sub.2 --CNor its hydrochloride, the improvement which comprises introducing aminoacetonitrile or its hydrochloride into a mixture of its chlorination products, with simultaneous addition of chlorine gas, in the absence of a solvent, at a temperature from about 70.degree. to 150.degree. C. The product can be further chlorinated at 130.degree. to 220.degree. C. to produce tetrachloro-ethylene-bis-isocyanide dichloride.
摘要翻译： 在制备式“IMAGE”的氯代N-甲基 - 咪唑和N-甲基 - 咪唑啉的制备中，其中n代表数字0,1,2或3，m表示数字0或1，双键存在于 当m为0时，4位和5位的C原子，当m为1时存在单键，通过氯化式（CH3）2N-CH2-CN或其盐酸盐的N，N-二甲基氨基乙腈， 其改进包括将氨基乙腈或其盐酸盐引入其氯化产物的混合物中，在约70-150℃的温度下，在不存在溶剂的情况下同时加入氯气。产物可以进一步在 130℃〜220℃，生成四氯 - 乙烯 - 双 - 异氰酸酯二氯化物。
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