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    Tricyclopentadienyl cerium and process for preparing the same
    13.
    发明授权
    Tricyclopentadienyl cerium and process for preparing the same 失效
    三环戊二烯基铈及其制备方法

    公开(公告)号：US4703109A

    公开(公告)日：1987-10-27

    申请号：US674639

    申请日：1984-11-26

    Applicant: Peter S. Gradeff ,  Fred G. Schreiber

    Inventor： Peter S. Gradeff ,  Fred G. Schreiber

    IPC: C07F5/00 ,  C07F17/00

    CPC classification number: C07F5/00

    Abstract: A process is provided for preparing tricyclopentadienyl cerium as well as the mono and dicyclopentadienyl cerium intermediates which comprises reacting an alkali metal cyclopentadienide with ceric ammonium nitrate, in solution in an inert organic solvent in a manner to obtain either tricyclopentadienyl cerium or to form in sequence, and stepwise, monocyclopentadienyl cerium dinitrate, dicyclopentadienyl cerium mononitrate, and tricyclopentadienyl cerium, depending upon the order of addition of the reactants.

    Abstract translation: 提供了制备三环戊二烯基铈以及单环和二环戊二烯基铈中间体的方法，其包括使碱金属环戊二烯与硝酸铈铵在溶液中在惰性有机溶剂中以获得三环戊二烯基铈或依次形成的方式进行反应， 和逐步的单环戊二烯二硝酸铈硝酸盐，二环戊二烯基一硝酸铈一硝酸铈和三环戊二烯基铈，这取决于反应物的添加顺序。

    Process for the preparation of ceric alkoxides
    14.
    发明授权
    Process for the preparation of ceric alkoxides 失效
    制备二氧化铈的方法

    公开(公告)号：US4663439A

    公开(公告)日：1987-05-05

    申请号：US674640

    申请日：1984-11-26

    Applicant: Peter S. Gradeff ,  Fred G. Schreiber

    Inventor： Peter S. Gradeff ,  Fred G. Schreiber

    IPC: C07C29/68 ,  C07C27/00 ,  C07C29/70 ,  C07C31/28 ,  C07C67/00 ,  C07F5/00

    CPC classification number: C07C29/70 ,  C07C31/28 ,  C07F5/003

    Abstract: A process is provided for preparing ceric alkoxides, which comprises reacting ceric ammonium nitrate complexed with and in solution in ethylene or propylene glycol ether or tetrahydrofuran with an anhydrous alkali metal alkoxide at a temperature within the range from about -30.degree. C. to about 200.degree. C., preferably from 0.degree. to about 150.degree. C., until ceric alkoxide and the nitrate salt of the base are formed; the nitrate formed during the reaction is insoluble in the glycol ether and tetrahydrofuran and can be separated from the reaction mixture, and the cerium alkoxide when soluble in the glycol ether or tetrahydrofuran can be isolated from the solution pure, or as the complex with the alcohol or with the solvent, or in some cases the alkoxide can be used without separation from the reaction mixture in the presence of the nitrate.

    Abstract translation: 提供了一种制备二氧化铈的方法，其包括使与乙烯或丙二醇醚或四氢呋喃中的溶液中的和硝酸铈配合的硝酸铈铵与无水碱金属醇盐在约-30℃至约200℃的温度下反应 优选0℃至约150℃，直到形成了铈醇盐和碱的硝酸盐; 反应过程中形成的硝酸盐不溶于乙二醇醚和四氢呋喃，可与反应混合物分离，可溶于乙二醇醚或四氢呋喃中的醇盐可以从溶液中纯化，或作为与醇的络合物 或在一些情况下，在硝酸盐存在下，可以不用分离反应混合物使用醇盐。

    Colloidal alcohol-dispersible association complexes of ceric dioxide and a hydroxyphenyl carboxylic acid
    16.
    发明授权
    Colloidal alcohol-dispersible association complexes of ceric dioxide and a hydroxyphenyl carboxylic acid 失效
    二氧化铈和羟基苯基羧酸的胶体醇分散缔合络合物

    公开(公告)号：US4886624A

    公开(公告)日：1989-12-12

    申请号：US87076

    申请日：1987-08-18

    Applicant: Peter S. Gradeff ,  Carlos Ramirez

    Inventor： Peter S. Gradeff ,  Carlos Ramirez

    IPC: C09D7/12 ,  C01F17/00 ,  C07C59/52 ,  C07C65/03 ,  C07F5/00 ,  B01J13/00 ,  C09D3/26 ,  C09K11/07

    CPC classification number: C07F5/003 ,  B01J13/0026 ,  B01J13/0047 ,  C01F17/0018 ,  C01F17/0043 ,  C07C59/52 ,  C07C65/03

    Abstract: A process is provided for preparing colloidal dispersions of alcohol-dispersible association complexes of ceric dioxide and a hydroxyphenyl carboxylic acid having from about seven to about twenty carbon atoms in a molar ratio CeO.sub.2 /acid of at least about 6:1 which comprises:(1) mixing(a) ceric dioxide comprising ammonium nitrate or ammonium and nitrate ions in an amount within the range from about 3 to about 14% by weight of the ceric dioxide and a member selected from the group consisting of water, methanol, acetic acid and mixtures thereof in an amount usually from about 10 to about 60 g per mole of CeO.sub.2, sufficient to effect reaction with(b) a hydroxyphenyl carboxylic acid having from about seven to about twenty carbon atoms(c) an aliphatic alcohol, such as methanol, isopropanol, 2-ethoxy ethanol, etc.at a temperature within the range from room temperature to about 100.degree. C., thereby effecting dispersion of the ceric dioxide in the aliphatic alcohol.

    Abstract translation: 提供了一种制备具有至少约6:1的摩尔比CeO 2 /酸的具有约7至约20个碳原子的二氧化铈和羟基苯基羧酸的醇可分散缔合络合物的胶体分散体的方法，其包括：（1 ）混合（a）包含硝酸铵或铵和硝酸根离子的二氧化铈，其量为二氧化铈的约3至约14重量％，以及选自水，甲醇，乙酸和 其混合物的量通常为每摩尔CeO 2约10至约60g，足以与（b）具有约7至约20个碳原子的羟基苯基羧酸反应（c）脂族醇如甲醇， 异丙醇，2-乙氧基乙醇等，在室温至约100℃的温度范围内，从而使二氧化铈在脂族醇中分散。

    Process for the preparation of hydroxy benzene carboxaldehydes
    17.
    发明授权
    Process for the preparation of hydroxy benzene carboxaldehydes 失效

    公开(公告)号：US4351962A

    公开(公告)日：1982-09-28

    申请号：US168940

    申请日：1980-07-11

    Applicant: Peter S. Gradeff ,  Stanley T. Murayama

    Inventor： Peter S. Gradeff ,  Stanley T. Murayama

    IPC: C07C37/20 ,  C07C45/38 ,  C07C45/80 ,  C07C45/81 ,  C07C45/82 ,  C07C45/36 ,  C07C45/00

    CPC classification number: C07C45/80 ,  C07C37/20 ,  C07C45/38 ,  C07C45/81 ,  C07C45/82 ,  Y02P20/582

    Abstract: A process is provided for the preparation of hydroxy benzene carboxaldehydes having the formula: ##STR1## wherein: R is selected from the group consisting of alkyl, alkoxy, cycloalkyl, aryl, alkoxyalkyl, fluoroalkyl, and hydroxyalkyl oxyalkylene having from one to about twenty carbon atoms; hydroxyalkyl having at least two to about twenty carbon atoms; hydroxy; aldehyde CHO; and halogen;n.sub.1, n.sub.2 and n.sub.3 are zero or 1; and at least one of n.sub.1, n.sub.2 and n.sub.3 is 1; andx is zero, 1, 2, 3 or 4, which comprises:(1) condensing with a formaldehyde compound a phenol having the formula: ##STR2## wherein R is selected from the group consisting of alkyl, alkoxy, hydroxyalkyl, cycloalkyl, aryl, alkoxyalkyl, fluoroalkyl, and hydroxyalkyl oxyalkylene having from one to about twenty carbon atoms; hydroxy; and halogen; andx is zero, 1, 2, 3 or 4,and unsubstituted in at least one ortho or para position in an aqueous reaction medium comprising phenol:HCHO in a molar ratio within the range from about 1:0.1 to about 1:3 and alkali in a molar ratio alkali:phenol within the range from about 1:0.1 to about 1:2 and an alkali concentration not exceeding 30% by weight at a temperature within the range from about 0.degree. to about 120.degree. C. and obtaining a reaction mixture comprising a mixture of monomethylol and polymethylol phenols having the formula: ##STR3## wherein R is selected from the group consisting of alkyl, alkoxy, hydroxyalkyl, cycloalkyl, aryl, alkoxyalkyl, fluoroalkyl, and hydroxyalkyl oxyalkylene having from one to about twenty carbon atoms; hydroxy; and halogen;n.sub.1, n.sub.2 and n.sub.3 are zero or 1; and at least one of n.sub.1, n.sub.2 and n.sub.3 is 1; andx is zero, 1, 2, 3 or 4;(2) subjecting the reaction mixture without separation of the monomethylol species from polymetholol species to oxidation under conditions favoring oxidation of methylol species to the corresponding aldehyde species in the presence of oxygen and an amount of alkali that is at least stoichiometrically equal to the amount of phenol and a platinum or palladium oxidation catalyst, preferably but optionally with a promoter selected from the group consisting of bismuth, lead, silver, tellurium, cadmium, and tin in the form of the metal and/or compounds thereof at a temperature within the range from about 0.degree. to about 100.degree. C. and a pH within the range from about 11 to about 13.5; and then(3) separating and recovering the desired aldehyde in the reaction mixture.A process also is provided for selectively decarbonylating any undesired aldehyde species to remove all or selected aldehyde groups in certain ring positions, either to yield more desirable aldehyde species or for recycling as starting material.

    Process for producing meta-phenoxybenzoic acids and esters
    18.
    发明授权
    Process for producing meta-phenoxybenzoic acids and esters 失效
    间苯氧基苯甲酸和酯的制备方法

    公开(公告)号：US4314070A

    公开(公告)日：1982-02-02

    申请号：US149588

    申请日：1980-05-14

    Applicant: Fred G. Schreiber ,  Peter S. Gradeff

    Inventor： Fred G. Schreiber ,  Peter S. Gradeff

    IPC: B01J27/00 ,  C07C65/21 ,  C07C69/92

    CPC classification number: C07C65/21 ,  C07C69/92

    Abstract: An improved process for producing meta-phenoxy benzoic acids and their lower alkyl esters in improved yields and with higher selectivity by reacting an alkali metal phenate with a lower alkyl ester of meta-halobenzoic acid in the presence of a copper sulfate catalyst.

    Abstract translation: 在硫酸铜催化剂存在下，通过使碱金属酚盐与间 - 卤代苯甲酸的低级烷基酯反应，以改进的产率和较高选择性制备间苯氧基苯甲酸及其低级烷基酯的改进方法。

    Process for preparing allylic alcohols from allylic halides
    20.
    发明授权
    Process for preparing allylic alcohols from allylic halides 失效
    从烯丙基卤化物制备烯丙醇的方法

    公开(公告)号：US4152530A

    公开(公告)日：1979-05-01

    申请号：US927330

    申请日：1978-07-24

    Applicant: Peter S. Gradeff

    Inventor： Peter S. Gradeff

    IPC: C07C27/02 ,  B01J27/00 ,  B01J31/00 ,  C07B61/00 ,  C07C27/00 ,  C07C29/09 ,  C07C33/02 ,  C07C67/00 ,  C07C29/00

    CPC classification number: C07C29/095 ,  C12C11/02

    Abstract: A process for preparing allylic alcohols from allylic halides is provided by way of the intermediate formation of an ester in the presence of a water-insoluble ketone forming an azeotrope in water followed by saponification of the ester with alkali metal hydroxide, drying the alkali metal carboxylic acid salt formed during the saponification by azeotropic distillatiion with the ketone, thus obviating expensive separate recovery facilities and handling of the dried alkali metal carboxyolate salt. The overall process amounts to a hydrolysis of the allylic halide with aqueous alkali metal hydroxide and one reactor can serve for the whole process.

    Abstract translation: 通过在水中形成共沸物的水不溶性酮的存在下中间形成酯，然后用碱金属氢氧化物皂化酯，提供由烯丙基卤制备烯丙醇的方法，干燥碱金属羧酸 通过与酮共沸蒸馏皂化期间形成的酸盐，从而避免了昂贵的分离回收设施和干燥的碱金属羧酸盐的处理。 总体方法相当于碱金属氢氧化物水溶液中的烯丙基卤化物水解，一个反应器可用于整个过程。

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