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    Process for the preparation of 2-nitrobenzaldehyde
    101.
    发明授权
    Process for the preparation of 2-nitrobenzaldehyde 失效
    制备2-硝基苯甲醛的方法

    公开(公告)号：US3996289A

    公开(公告)日：1976-12-07

    申请号：US557297

    申请日：1975-03-11

    Applicant: Horst Meyer

    Inventor： Horst Meyer

    IPC: C07C205/44 ,  A61K31/04 ,  A61K31/11 ,  C07B41/06 ,  C07C20060101 ,  C07C27/00 ,  C07C47/54 ,  C07C51/16 ,  C07C67/00 ,  C07C201/00 ,  C07C201/12 ,  C07D211/82

    CPC classification number: C07C205/44 ,  C07C201/12

    Abstract: 2-NITROBENZALDEHYDE, A VALUABLE CHEMICAL INTERMEDIATE, IS PREPARED THROUGH THE OXIDATION OF AN ALKALI METAL SALT OF 2-NITROPHENYLPYRUVIC ACID WITH POTASSIUM PERMANGANATE IN AN ALKALINE MEDIUM. Advantageously the requisite starting material is prepared directly by the reaction of 2-nitrotoluene and a diester of oxalic acid in the presence of an alcoholate and is then subjected to the oxidation without isolation. In a preferred embodiment the oxidation reaction mixture is acidified to convert the manganese-(IV) oxide to soluble maganese-(II) salts with concurrent conversion of oxalic acid to carbon dioxide. The process is industrially attractive in terms of the high yield, the availability of starting material and the ease of the manipulative steps involved.

    Abstract translation: 2-NITROBENZALDEHYDE，一种有价值的化学中间体，是通过在碱性介质中用硫酸钾处理2-硝基戊酸的碱金属盐来制备的。 有利的是，必需的原料直接通过在醇化物存在下由2-硝基甲苯与草酸二酯的反应制备，然后在不分离的条件下进行氧化。 在优选的实施方案中，将氧化反应混合物酸化以将锰（IV）氧化物转化为可溶性的锰 - （II）盐，同时将草酸转化为二氧化碳。 该方法在高产率，起始材料的可用性和所涉及的操纵步骤的容易性方面在工业上具有吸引力。

    Dinitration of nitrobenzotrifluoride
    103.
    发明授权
    Dinitration of nitrobenzotrifluoride 失效
    二硝基三氟甲苯的硝化

    公开(公告)号：US3984488A

    公开(公告)日：1976-10-05

    申请号：US580505

    申请日：1975-05-23

    Applicant: Barton Milligan

    Inventor： Barton Milligan

    IPC: C07C67/00 ,  C07C201/00 ,  C07C205/11 ,  C07C205/12 ,  C07C205/58 ,  C07C79/12

    CPC classification number: C07C201/12

    Abstract: This invention relates to an improvement in an process for dinitrating 3-nitrobenzotrifluoride and 4-hal0-3-nitrobenzotrifluoride compounds wherein the mononitrobenzotrifluoride composition is contacted with a mixture comprising sulfuric and nitric acid. The improvement constituting the basis of this invention comprises carrying out the dinitration with the sulfuric acid being present in at least a catalytic proportion but not exceeding about 65 mole percent in said mixture.

    Abstract translation: 本发明涉及三硝基三氟甲苯和4-卤代-3-硝基三氟甲苯化合物的二硝化方法的改进，其中一硝基三氟甲苯组合物与包含硫酸和硝酸的混合物接触。 构成本发明基础的改进包括以所述混合物中至少催化比例但不超过约65摩尔％的硫酸进行二硝化。

    Method for making certain halonium salt photoinitiators
    105.
    发明授权
    Method for making certain halonium salt photoinitiators 失效
    制备某些卤盐光引发剂的方法

    公开(公告)号：US3981897A

    公开(公告)日：1976-09-21

    申请号：US574007

    申请日：1975-05-02

    Applicant: James V. Crivello

    Inventor： James V. Crivello

    IPC: C08F2/00 ,  C07C17/00 ,  C07C17/35 ,  C07C25/02 ,  C07C25/18 ,  C07C67/00 ,  C07C201/00 ,  C07C205/12 ,  C07F9/90 ,  C08F2/50 ,  C08G59/00 ,  C08G59/68 ,  G03F7/029 ,  C07F9/66

    CPC classification number: C07F9/902 ,  C08G59/68 ,  G03F7/029

    Abstract: A method is provided for making certain diarylhalonium salts containing Group Va metal hexafluorides useful as photoinitiators, such as diphenyliodonium hexafluoroarsonate. An intermediate diarylhalonium bisulfate is prepared. Reaction is thereafter effected between the diarylhalonium bisulfate and the source of a counterion, such as AsF.sub.6 .sup.- , in the form of the corresponding acid or salt. The halonium salt photoinitiators can be used to make UV curable compositions.

    Abstract translation: 提供了一种制备含有可用作光引发剂的第Va族金属六氟化铬的某些二芳基卤鎓盐的方法，例如六氟砷酸二苯基碘鎓。 制备中间体二芳基脲硫酸氢盐。 此后，以相应的酸或盐的形式在二硫酸氢二铵和抗衡离子源（如AsF 6 - ）之间进行反应。 卤盐光引发剂可用于制备紫外光固化组合物。

    Process for preparing 1-nitro-anthraquinone
    107.
    发明授权
    Process for preparing 1-nitro-anthraquinone 失效
    1-硝基 - 蒽醌的制备方法

    公开(公告)号：US3960903A

    公开(公告)日：1976-06-01

    申请号：US501017

    申请日：1974-08-27

    Applicant: Karl Linhart ,  Reinold Schmitz

    Inventor： Karl Linhart ,  Reinold Schmitz

    IPC: C07C205/47 ,  C07C20060101 ,  C07C67/00 ,  C07C201/00 ,  C07C49/68

    CPC classification number: C07C205/47

    Abstract: 1-Nitro-anthraquinone is separated from an anthraquinone nitration mixture in concentrated nitric acid by adding to the nitration mixture sulpholan and separating off the insoluble 1-nitro-anthraquinone. The quantity of sulpholan added is such that the mixture contains 10-90% by weight nitric acid and from 90-10% by weight sulpholan.

    Abstract translation: 将1-硝基蒽醌与浓硝酸中的蒽醌硝化混合物分离，加入到硝化混合物溶液中，分离出不溶性的1-硝基蒽醌。 所添加的sulpholan的量使得混合物含有10-90重量％的硝酸和90-10重量％的sulpholan。

    Recovery of polymerization inhibitor
    108.
    发明授权
    Recovery of polymerization inhibitor 失效
    回收阻聚剂

    公开(公告)号：US3959395A

    公开(公告)日：1976-05-25

    申请号：US536271

    申请日：1974-12-26

    Applicant: Thomas D. Higgins, Jr. ,  Raymond A. Newsom

    Inventor： Thomas D. Higgins, Jr. ,  Raymond A. Newsom

    IPC: C07C7/04 ,  C07C1/00 ,  C07C7/20 ,  C07C15/44 ,  C07C15/46 ,  C07C67/00 ,  C07C201/00 ,  C07C201/16 ,  C07C205/22 ,  C07C205/23 ,  C07C79/24 ,  C07C37/28

    CPC classification number: C07C201/16 ,  C07C7/20

    Abstract: A process is provided for recovery and re-use of dinitrophenols employed as inhibitors of polymerization in the distillation and purification of styrene. The styrene still residues commonly referred to as tar or tars are treated with an aqueous hydroxide at a controlled pH, the phases are separated, the aqueous phase is treated with an acid and an organic solvent at a controlled pH and the resulting organic phase is recycled to a suitable point in the styrene purification system. The recycled solution is a more effective inhibitor than the dinitrophenol originally employed.

    Abstract translation: 提供了一种在苯乙烯的蒸馏和纯化中用作聚合抑制剂的二硝基苯酚的回收和再利用方法。 通常被称为焦油或焦油的苯乙烯残留物在受控的pH下用氢氧化物水溶液处理，分离各相，水相在受控的pH下用酸和有机溶剂处理，并将所得的有机相回收 到苯乙烯净化系统中的合适点。 回收的溶液比起初使用的二硝基苯酚更有效。

    Process for preparing highly pure 5-nitro-1,4,4a,9a-tetrahydroanthraquinone
    109.
    发明授权
    Process for preparing highly pure 5-nitro-1,4,4a,9a-tetrahydroanthraquinone 失效
    制备高纯度5-硝基-1,4,4a，9a-四氢蒽醌的方法

    公开(公告)号：US3959318A

    公开(公告)日：1976-05-25

    申请号：US610778

    申请日：1975-09-05

    Applicant: Yasuyoshi Torisu ,  Seishichiro Kaba ,  Ken Mukai

    Inventor： Yasuyoshi Torisu ,  Seishichiro Kaba ,  Ken Mukai

    IPC: C07C205/47 ,  C07C67/00 ,  C07C201/00 ,  C07C205/45 ,  C07C49/68

    CPC classification number: C07C201/12 ,  C07C205/47 ,  C07C221/00 ,  C07C2103/24

    Abstract: Highly pure 5-nitro-1,4,4a,9a-tetrahydroanthraquinone can be obtained by subjecting 6-nitronaphthoquinone-containing crude 5-nitro-1,4-naphthoquinone to Diels-Alder condensation reaction with 1,3-butadiene in a solvent including benzene, an alkylated aromatic hydrocarbon such as toluene, xylene or the like, a halogenated aromatic hydrocarbon such as chlorobenzene, dichlorobenzene, or the like, or a halogenated aliphathic hydrocarbon such as trichloroethylene, perchloroethylene or the like, cooling the resulting reaction solution to crystallize the reaction product, and separating the thus crystallized product by filtration. 5-nitro-1,4,4a,9a-tetrahydroanthraquinone has a relatively small solubility in the above-mentioned solvents, while the solubility of 6-nitro-1,4,4a,9a-tetrahydroanthraquinone in the solvents is rather great, thus the above-mentioned solvents being effective for the separation of these compounds from each other. The oxidation and the subsequent reduction of the thus obtained 5-nitro-1,4,4a,9a-tetrahydroanthraquinone yields 1-aminoanthraquinone with a purity above 98 wt% and a 2-aminoanthraquinone content below 1 wt%. The above-mentioned solvents are also effective for purification of 6-nitro-1,4,4a,9a-tetrahydroanthraquinone-containing 5-nitro-1,4,4a,9a-tetrahydroanthraquinone by recrystallization.

    Abstract translation: 通过使6-硝基萘醌的粗5-硝基-1,4-萘醌与溶剂中的1,3-丁二烯进行狄尔斯 - 阿尔德缩合反应，可以得到高纯度的5-硝基-1,4,4a，9a-四氢蒽醌 包括苯，烷基化芳烃如甲苯，二甲苯等，卤代芳烃如氯苯，二氯苯等，或卤代脂族烃如三氯乙烯，全氯乙烯等，将所得反应溶液冷却至 使反应产物结晶，并通过过滤分离如此结晶的产物。 5-硝基-1,4,4a，9a-四氢蒽醌在上述溶剂中的溶解度相对较小，而6-硝基-1,4,4a，9a-四氢蒽醌在溶剂中的溶解度相当大，因此 上述溶剂对于将这些化合物彼此分离是有效的。 由此得到的5-硝基-1,4,4a，9a-四氢蒽醌的氧化和随后的还原得到纯度高于98wt％，2-氨基蒽醌含量低于1wt％的1-氨基蒽醌。 上述溶剂对于通过重结晶纯化含有6-硝基-1,4,4a，9a-四氢蒽醌的5-硝基-1,4,4a，9a-四氢蒽醌也是有效的。

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