Process for the preparation of cinnamic acids which are optionally
substituted in the nucleus
    1.
    发明授权
    Process for the preparation of cinnamic acids which are optionally substituted in the nucleus 失效
    在核中任选取代的肉桂酸的制备方法

    公开(公告)号:US4613692A

    公开(公告)日:1986-09-23

    申请号:US743254

    申请日:1985-06-11

    CPC分类号: C07C51/353

    摘要: A process for the preparation of cinnamic acid is provided by the present invention in which an optionally substituted benzaldehyde and alkali metal salt of carboxylic acid and/or alkali metal (bi) carbonate, as condensing agents, are heated up to a temperature of 100.degree.-220.degree. C. and thereafter there is introduced into the so heated mixture acetic anhydride in at least a stoichiometric amount based upon the amount of optionally substituted benzaldehyde employed. The process can be carried out by heating up a reaction mixture to 100.degree.-220.degree. C. which is free of acetic anhydride or one which contains acetic anhydride but less than a stoichiometric amount thereof based upon the amount of optionally substituted benzaldehyde.

    摘要翻译: 通过本发明提供了制备肉桂酸的方法,其中将任选取代的苯甲醛和羧酸和/或碱金属(bi)碳酸盐的碱金属盐作为缩合剂加热至100℃ -220℃,然后基于所使用的任选取代的苯甲醛的量,以至少化学计量的量将如此加热的混合物乙酸酐引入。 该方法可以通过将反应混合物加热至不含乙酸酐的100℃-220℃或基于任选取代的苯甲醛的量而含有乙酸酐但少于其化学计量的反应混合物进行。

    5,5-dichloro-4,5-dihydro-6-hydroxy-2-trichloromethylpyrimidin-4-one
    2.
    发明授权
    5,5-dichloro-4,5-dihydro-6-hydroxy-2-trichloromethylpyrimidin-4-one 失效
    5,5-二氯-4,5-二氢-6-羟基-2-三氯甲基嘧啶-4-酮

    公开(公告)号:US4668788A

    公开(公告)日:1987-05-26

    申请号:US766586

    申请日:1985-08-19

    CPC分类号: C07D239/30 C07D239/553

    摘要: The new compound 5,5-dichloro-4,5-dihydro-6-hydroxy-2-trichloromethylpyrimidin-4-one can be prepared by reacting 4,6-dihydroxy-2-methylpyrimidine or chlorinated subsequent stages with a chlorinating agent. 5,5-dichloro-4,5-dihydro-6-hydroxy-2-trichloromethylpyrimidin-4-one can be used as an intermediate for the preparation of 2-trichloromethyl-4,5,6-trichloropyrimidine.

    摘要翻译: 新化合物5,5-二氯-4,5-二氢-6-羟基-2-三氯甲基嘧啶-4-酮可以通过使4,6-二羟基-2-甲基嘧啶或氯化后续阶段与氯化剂反应来制备。 5,5-二氯-4,5-二氢-6-羟基-2-三氯甲基嘧啶-4-酮可以用作制备2-三氯甲基-4,5,6-三氯嘧啶的中间体。

    1,3-di-arylmethoxy-4,6-dinitro-benzenes, process for their preparation
and process for the preparation of 4,6-diaminoresorcinol
    4.
    发明授权
    1,3-di-arylmethoxy-4,6-dinitro-benzenes, process for their preparation and process for the preparation of 4,6-diaminoresorcinol 失效
    1,3-二氨基四甲基-4,6-二苯乙烯,其制备方法和制备4,6-DIAMINORESORCINOL的方法

    公开(公告)号:US5072053A

    公开(公告)日:1991-12-10

    申请号:US526357

    申请日:1990-05-21

    CPC分类号: C07C205/37 C07C213/02

    摘要: The new 1,3-di-arylmethoxy-4,6-dinitrobenzenes of the formula ##STR1## in which R.sup.1 and R.sup.2 independently of one another denote hydrogen or C.sub.1 -C.sub.4 -alkyl andAr represents C.sub.6 -C.sub.12 -aryl,can be prepared by reaction of 1,3-dihalogeno-4,6-dinitro-benzenes of the formula ##STR2## in which Hal represents chlorine or bromine, with an arylmethanol of the formulaAr--C(R.sup.1, R.sup.2)OH (IV),in which R.sup.1, R.sup.2 and Ar have the said meaning, and a strong base in the temperature range from 0.degree. to 100.degree. C.These di-arylmethoxy-dinitro-benzenes can be converted into 4,6-diaminoresorcinol by catalytic reduction with hydrogen.

    摘要翻译: 式(Ⅰ)的新的1,3-二芳基甲氧基-4,6-二硝基苯,其中R 1和R 2彼此独立地表示氢或C 1 -C 4烷基,Ar表示C 6 -C 12 - 芳基, 可以通过式(III)的1,3-二卤代-4,6-二硝基苯(其中Hal表示氯或溴)与式Ar-C的芳基甲醇(R1,R2 )OH(IV),其中R1,R2和Ar具有所述含义,在0℃至100℃的温度范围内具有强碱。这些二芳基甲氧基 - 二硝基苯可以转化为4,6- 用氢气催化还原二氨基间苯二酚。

    Process for the purification of nitrobenzaldenhyde
    5.
    发明授权
    Process for the purification of nitrobenzaldenhyde 失效
    硝基苯甲醛的纯化方法

    公开(公告)号:US4910345A

    公开(公告)日:1990-03-20

    申请号:US231740

    申请日:1988-08-12

    CPC分类号: C07C201/16

    摘要: Crude nitrobenzaldehyde can be substantially purified from the undesired positional isomers if a treatment with 100-10,000% by weight of water and 1-30% by weight of an emulsifier, all with reference to the dry weight of the crude nitrobenzaldehyde, is undertaken at a temperature of 30.degree.-140.degree. C. and at a pH of 3-14.

    摘要翻译: 如果使用100-10,000重量%的水和1-30重量%的乳化剂处理,全部参照粗制硝基苯甲醛的干重,就可以从不希望的位置异构体中纯化粗硝基苯甲醛。 温度为30°-140℃,pH为3-14。

    Process for preparing acid halides
    6.
    发明授权
    Process for preparing acid halides 失效
    制备酰卤的方法

    公开(公告)号:US4863642A

    公开(公告)日:1989-09-05

    申请号:US396513

    申请日:1982-07-08

    CPC分类号: C07C51/58

    摘要: Acid halides of the formula (R.sup.1, R.sup.2, R.sup.3)C--CO--Hal are obtained by reacting alkyl halides of the formula (R.sup.1, R.sup.2, R.sup.3)C--Hal with carbon monoxide under a pressure of 5 to 1,000 bar and at a temperature of -20.degree. C. to +100.degree. C. in the presence of 0.001 to 0.3 mol of AlCl.sub.3 and/or FeCl.sub.3, if appropriate in the presence of a further Bronsted or Lewis acid, per mol of the alkyl halide. The process is carried out, if desired in the presence of a solvent which is customary for Friedel-Crafts or Friedel-Crafts-related reactions and, if appropriate in the presence of a hydrogen halide. The acid chloride can be isolated from the reaction mixture or further reacted.

    摘要翻译: 式(R1,R2,R3)C-CO-Hal的酰卤由式(R1,R2,R3)C-Hal的烷基卤与一氧化碳在5〜1000巴的压力下反应而获得, 在0.001至0.3mol AlCl 3和/或FeCl 3的存在下,如果合适,在另外的布朗斯台德或路易斯酸存在下,每摩尔烷基卤化物在-20℃至+ 100℃的温度下进行。 如果需要,在通常用于Friedel-Crafts或Friedel-Crafts相关反应的溶剂存在下,并且如果合适的话,在卤化氢存在下进行该方法。 酰氯可以从反应混合物中分离出来或进一步反应。

    Process for the preparation of 3-hydroxybenzoic acid
    7.
    发明授权
    Process for the preparation of 3-hydroxybenzoic acid 失效
    3-羟基苯甲酸的制备方法

    公开(公告)号:US4393234A

    公开(公告)日:1983-07-12

    申请号:US378922

    申请日:1982-05-17

    CPC分类号: C07C309/00 C07C51/367

    摘要: 3-Hydroxybenzoic acid is obtained by reaction with an alkali metal hydroxide at a temperature of 220.degree. to 450.degree. C. and under a pressure of 1 to 120 bars, from a technical 3-sulphobenzoic acid mixture which contains sulphuric acid and/or sulphur trioxide and which contains at least 75% by weight of 3-sulphobenzoic acid, relative to the total organic constituents present, and not more than 35% by weight of sulphuric acid and/or SO.sub.3, relative to the total mass. For this purpose, this technical 3-sulphobenzoic acid mixture, if desired after dilution with an equal volume of water, is mixed with sufficient 50 to 100% strength by weight alkali metal hydroxide wherein the remaining 50 to 0% by weight consists essentially of water, for 2.5 to 8 mols of alkali metal hydroxide to be present per mol of 3-sulphobenzoic acid, after neutralization of the sulphuric acid and all the sulpho and carboxyl groups. In general, 10 to 45% by weight of water are present in the batch. The reaction mixture is acidified with a mineral acid to a pH value of less than 4, if appropriate after dilution with water, and the 3-hydroxybenzoic acid is isolated at temperatures within the range from -5.degree. C. to +40.degree. C.

    摘要翻译: 通过在含有硫酸和/或硫的工业3-磺基苯甲酸混合物的温度在220-450℃和1至120巴的压力下与碱金属氢氧化物反应获得3-羟基苯甲酸 三氧化硫,相对于存在的总有机成分含有至少75重量%的3-磺基苯甲酸,相对于总质量不超过35重量%的硫酸和/或SO 3。 为此目的,如果需要,在等体积水稀释后,将该技术性3-磺基苯甲酸混合物与足量的50至100%重量的碱金属氢氧化物混合,其中剩余的50至0重量%基本上由水 对于每摩尔3-磺基苯甲酸存在的2.5至8摩尔碱金属氢氧化物,中和硫酸和所有磺基和羧基后。 通常,批料中存在10至45重量%的水。 如果在用水稀释后,将反应混合物用无机酸酸化至pH值小于4,并且在-5℃至+ 40℃的温度下分离出3-羟基苯甲酸。

    Process for the delignification of lignocellulose materials with
dinitroanthraquinones
    8.
    发明授权
    Process for the delignification of lignocellulose materials with dinitroanthraquinones 失效
    木质纤维素材料与二硝基蒽醌脱木质素的方法

    公开(公告)号:US4350566A

    公开(公告)日:1982-09-21

    申请号:US257842

    申请日:1981-04-27

    CPC分类号: D21C3/222

    摘要: A process for delignifying lignocellulosic material with a digestion liquor of nitroanthraquinones and/or dinitroanthraquinones. The process can be carried out in a closed reaction vessel at temperatures of 150.degree.-200.degree..+-. C. for 0.5 to 480 minutes with 0.001 to 10% nitroanthraquinone and/or dinitroanthraquinone by weight of lignocellulosic material.

    摘要翻译: 用硝基蒽醌和/或二硝基蒽醌的消化液脱木质纤维素材料的方法。 该方法可以在封闭的反应容器中,在150-2200℃的温度下进行0.5至480分钟,其中0.001至10%的硝基蒽醌和/或二硝基蒽醌以木质纤维素材料的重量计。

    Preparation of .alpha.-ketocarboxylic acid N-tert.-butylamides
    9.
    发明授权
    Preparation of .alpha.-ketocarboxylic acid N-tert.-butylamides 失效
    α-酮羧酸N-叔丁基酰胺的制备

    公开(公告)号:US4345100A

    公开(公告)日:1982-08-17

    申请号:US222222

    申请日:1981-01-02

    CPC分类号: C07D253/075

    摘要: A process for the preparation of an .alpha.-ketocarboxylic acid N-tert.-butylamide of the formulaR--CO--CO--NH--C(CH.sub.3).sub.3in whichR is an aliphatic radical with up to 8 carbon atoms, a cycloalkyl radical with 3 to 6 carbon atoms, a phenyl or naphthyl radical or a heterocyclic radical,comprising reacting an acyl cyanide of the formulaR--CO--CNwith tert.-butyl methyl ether of the formula(CH.sub.3).sub.3 C--O--CH.sub.3at a temperature between about 0.degree. and 80.degree. C. in the presence of an acid which is capable of activating the ether of formula (III) under the reaction conditions to give a tert.-butyl carbonium ion, and then hydrolyzing the reaction mixture. Advantageously the acyl cyanide is pivaloyl cyanide or benzoyl cyanide and is reacted with an approximately equimolar amount of the ether in the presence of about 1.1 to 1.5 times the molar amount of concentrated sulphuric acid as the activating acid. The products are useful as intermediates in the synthesis of known herbicides.

    摘要翻译: 制备式R-CO-CO-NH-C(CH3)3的α-酮羧酸N-叔丁基酰胺的方法,其中R是具有至多8个碳原子的脂族基团,环烷基 具有3至6个碳原子,苯基或萘基或杂环基,其包括使式R-CO-CN的酰基氰与式(CH 3)3 C-O-CH 3的叔丁基甲基醚在 在能够在反应条件下活化式(III)的醚的酸存在下,温度在约0℃至80℃之间,得到叔丁基碳鎓离子,然后水解反应混合物。 有利地,酰基氰是新戊酰氰或苯甲酰氰,并且在作为活化酸的浓硫酸的摩尔量的约1.1至1.5倍的存在下,与约等摩尔量的醚反应。 该产品可用作合成已知除草剂的中间体。