Process for preparing substituted aromatic and heteroaromatic aldehydes and carboxylic acids
    1.
    发明授权
    Process for preparing substituted aromatic and heteroaromatic aldehydes and carboxylic acids 失效
    取代的芳族和杂芳族醛和羧酸的制备方法

    公开(公告)号:US06518455B1

    公开(公告)日:2003-02-11

    申请号:US09473020

    申请日:1999-12-28

    IPC分类号: C07C30900

    摘要: A process for preparing substituted aromatic and heteroaromatic aldehydes or carboxylic acids of the formula in which R1 and R2 are H, C1-C4 alkyl, C1-C4 alkoxy, OH, NO2, CN, COOH, CONH2, COOR, NH2, SO3H or halogen and R is C1-C4 alkyl and where R1 and R2 are not simultaneously H, X is C or N and Z is CHO or COOH, from the corresponding symmetric stilbene compounds of the formula in which R1, R2 and X are as defined above, by aqueous ozonolysis and subsequent isolation of an aldehyde or oxidation to give the corresponding carboxylic acid.

    摘要翻译: R1和R2是H,C1-C4烷基,C1-C4烷氧基,OH,NO2,CN,COOH,CONH2,COOR,NH2,SO3H或卤素的取代芳族和杂芳族醛或羧酸的方法,以及 R是C1-C4烷基,其中R1和R2不同时为H,X为C或N,Z为CHO或COOH,R1,R2和X如上定义的式对应的对称二苯乙烯化合物, 臭氧分解并随后分离醛或氧化,得到相应的羧酸。

    Process for preparing high-purity, halogen-free o-phthaladehyde
    2.
    发明授权
    Process for preparing high-purity, halogen-free o-phthaladehyde 有权
    制备高纯度无卤素邻苯二甲醛的方法

    公开(公告)号:US07858381B2

    公开(公告)日:2010-12-28

    申请号:US11475086

    申请日:2006-06-27

    IPC分类号: G01N33/00

    摘要: Improved process for preparing high-purity, halogen-free o-phthalaldehyde, in which a) tetrahalo-o-xylene is hydrolyzed at a temperature of 155-160° C. and a pressure of from 2 to 5 bar, where appropriate in the presence of a phase-transfer catalyst, to o-phthalaldehyde, which b) is converted in an acidic alcoholic solution at a temperature of from 0 to the reflux temperature into the corresponding dialkoxyphthalane and, subsequently, c) an acetal cleavage is effected by acid hydrolysis at a pH >1.5 to pH 7, resulting in high-purity, halogen-free o-phthalaldehyde.

    摘要翻译: 改进的制备高纯度无卤邻苯二甲醛的方法,其中a)四卤代邻二甲苯在155-160℃的温度和2至5巴的压力下水解, 相转移催化剂存在于邻苯二甲醛中,b)在酸性醇溶液中在0至回流温度下转化成相应的二烷氧基苯烷,然后c)通过酸进行缩醛裂解 在pH> 1.5至pH7下水解,得到高纯度,无卤素的邻苯二甲醛。

    Process for the preparation of 2,3-pyridinedicarboxylic acids
    3.
    发明授权
    Process for the preparation of 2,3-pyridinedicarboxylic acids 失效
    2,3-吡啶二羧酸的制备方法

    公开(公告)号:US06395903B1

    公开(公告)日:2002-05-28

    申请号:US09569057

    申请日:2000-05-10

    IPC分类号: C07D21380

    CPC分类号: C07D213/80

    摘要: Process for the preparation of pure 2,3-pyridinedicarboxylic acids of the formula I which are substituted in position 4 and/or 5 and/or 6 by R1, where R1 is hydrogen, C1-C4 alkyl, C1-C4 alkoxy, C1-C4 alkoxy-C1-C4 alkyl, halogen, hydroxyl or nitro, from quinolines of the formula II in which R1 is as defined above, and which are substituted in position 6 and/or 7 by R2, where R2 is hydrogen, C1-C4 alkyl, C1-C4 alkoxy, C1-C4 alkoxy-C1-C4 alkyl, halogen, hydroxyl, nitro or amino, which are reacted in the first step in aqueous sulfuric acid or nitric acid solution with ozone in the ratio of from 1:2 to 1:3 at temperatures from 0 to +50° C., and the resulting peroxide solution is then reacted at temperatures of from +0 to +100° C. in the presence of 0.5-4.0 mol of oxidizing agent per mole of ozonolysis product formed, after which the pH of the reaction solution is adjusted to 0.2 to 3, the mixture is cooled to 0 to 30° C., and the precipitated pyridinedicarboxylic acid is isolated.

    摘要翻译: 制备式Ⅰ的纯的2,3-吡啶二羧酸的方法,其中R1是氢,C1-C4烷基,C1-C4烷氧基,C1-C4烷基, 烷氧基-C 1 -C 4烷基,卤素,羟基或硝基,其中R 1如上定义,并且其中R 2为氢,C 1 -C 4烷基,C 1 -C 4烷基, C 1 -C 4烷氧基,C 1 -C 4烷氧基-C 1 -C 4烷基,卤素,羟基,硝基或氨基,它们在第一步中在硫酸水溶液或硝酸溶液中与臭氧按1:2比1反应 :3,在0至+ 50℃的温度下,然后将所得过氧化物溶液在+ 0至+ 100℃的温度下在每摩尔臭氧分解产物0.5-4.0摩尔氧化剂存在下反应 之后,将反应溶液的pH调节至0.2〜3,将混合物冷却至0〜30℃,分离析出的吡啶二甲酸。

    Method for producing hydroxymethylpyridines
    7.
    发明授权
    Method for producing hydroxymethylpyridines 失效
    羟甲基吡啶的制备方法

    公开(公告)号:US06486327B1

    公开(公告)日:2002-11-26

    申请号:US10129189

    申请日:2002-05-02

    IPC分类号: C07D21304

    CPC分类号: C07D213/30

    摘要: The invention relates to a method for producing hydroxymethylpyridines from the corresponding vinylpyridines by means of ozonisation in an alcohol as solvent and by means of hydrogenation of the peroxide-containing solution produced thereby, in the presence of a hydrogenation catalyst The hydrogenation solution is adjusted to a pH value of 10 to 14 by adding a base and the alcohol is distilled off and the desired hydroxymethylpyridine is isolated in high purity by extracting with an organic solvent and by means of subsequent distillative purification.

    摘要翻译: 本发明涉及通过在醇作为溶剂中的臭氧化和通过在由氢化催化剂的存在下氢化产生的含过氧化物的溶液从对应的乙烯基吡啶生产羟甲基吡啶的方法。将氢化溶液调节至 通过加入碱将pH值降至10至14,并蒸除醇,通过用有机溶剂萃取并通过随后的蒸馏纯化将所需的羟甲基吡啶分离成高纯度。

    Process for preparing high-purity, halogen-free o-phthaladehyde
    9.
    发明申请
    Process for preparing high-purity, halogen-free o-phthaladehyde 有权
    制备高纯度无卤素邻苯二甲醛的方法

    公开(公告)号:US20060293542A1

    公开(公告)日:2006-12-28

    申请号:US11475086

    申请日:2006-06-27

    IPC分类号: C07C45/00

    摘要: Improved process for preparing high-purity, halogen-free o-phthalaldehyde, in which a) tetrahalo-o-xylene is hydrolyzed at a temperature of 155-160° C. and a pressure of from 2 to 5 bar, where appropriate in the presence of a phase-transfer catalyst, to o-phthalaldehyde, which b) is converted in an acidic alcoholic solution at a temperature of from 0 to the reflux temperature into the corresponding dialkoxyphthalane and, subsequently, c) an acetal cleavage is effected by acid hydrolysis at a pH >1.5 to pH 7, resulting in high-purity, halogen-free o-phthalaldehyde.

    摘要翻译: 改进的制备高纯度无卤邻苯二甲醛的方法,其中a)四卤代邻二甲苯在155-160℃的温度和2至5巴的压力下水解, 相转移催化剂存在于邻苯二甲醛中,b)在酸性醇溶液中在0至回流温度下转化成相应的二烷氧基苯烷,然后c)通过酸进行缩醛裂解 在pH> 1.5至pH7下水解,得到高纯度,无卤素的邻苯二甲醛。

    Process for the purification and formulation of o-phthalaldehyde
    10.
    发明授权
    Process for the purification and formulation of o-phthalaldehyde 失效
    邻苯二甲醛的纯化和配制方法

    公开(公告)号:US06486358B1

    公开(公告)日:2002-11-26

    申请号:US10144887

    申请日:2002-05-15

    IPC分类号: C07C4500

    摘要: Improved process for the purification and formulation of o-phthalaldehyde in which crude o-phthalaldehyde, obtained by cleavage of an acetal of o-phthalaldehyde by means of acidic hydrolysis, is, optionally by adding an aqueous basic solution, adjusted to a pH of from 1 to 8, and then, after phase separation has taken place, water is distilled off from the phase which contains the aldehyde with very short thermal stress of less than 1 minute at a pressure of between 100 mbar and atmospheric pressure and a temperature of from room temperature to 180° C. on a thin-layer overhead evaporator and o-phthalaldehyde is then stripped off from the distillation bottom which remains with very short thermal stress of less than 1 minute at a pressure of from 0.5 to 50 mbar and a jacket temperature of from 80 to 80° C. via a thin-layer evaporator and the resulting o-phthalaldehyde melt is pelleted at atmospheric pressure and a temperature of from 60 to 80° C., giving pale yellow o-phthalaldehyde in high purity and storage-stable form.

    摘要翻译: 用于纯化和制备邻苯二甲醛的改进方法,其中通过酸性水解裂解邻苯二甲醛的缩醛获得的粗邻苯二甲醛,任选地通过加入碱性水溶液,调节至pH为 1至8,然后在相分离发生后,在100 mbar和大气压之间的压力下,从包含醛的相中蒸出水,其热应力小于1分钟,热应力非常短 然后在薄层塔顶蒸发器上室温至180℃,然后从蒸馏塔底部除去邻苯二甲醛,蒸馏塔底部保持非常短的热应力,压力为0.5至50毫巴,夹套小于1分钟 通过薄层蒸发器温度为80至80℃,并将所得的邻苯二甲醛熔体在大气压和60至80℃的温度下沉淀,得到淡黄色邻苯二甲醛 n高纯度和储存稳定的形式。