公开(公告)号：US5527753A

公开(公告)日：1996-06-18

申请号：US354998

申请日：1994-12-13

申请人： John F. Engel ,  Conrad W. Kamienski ,  James A. Schwindeman ,  Randy W. Hall ,  Robert C. Morrison ,  B. Troy Dover

发明人： John F. Engel ,  Conrad W. Kamienski ,  James A. Schwindeman ,  Randy W. Hall ,  Robert C. Morrison ,  B. Troy Dover

IPC分类号： C08F4/46 ,  C08F4/48 ,  C08F12/04 ,  C08F36/04 ,  B01J31/12 ,  B01J31/18

CPC分类号： C08F12/04 ,  C08F36/04

摘要： A process for the preparation of hydrocarbon solutions of monofunctional amine initiators of the following general structures: ##STR1## wherein M is defined as an alkali metal, selected from the group consisting of lithium, sodium and potassium, Q is a saturated or unsaturated hydrocarbyl group derived by incorporation of a compound selected from the group consisting of conjugated diene hydrocarbons and alkenyl substituted aromatic hydrocarbons; Z is a hydrocarbon tether group which contains 3-25 carbon atoms; A is an element selected from Group IVa of the periodic table and R.sup.1, R.sup.2, and R.sup.3 are independently selected from hydrogen, alkyl, substituted alkyl, cycloalkyl, aryl or substituted aryl groups, m is an integer from 0 to 7, and n is an integer from 1 to 5, monofunctional amine initiators produced by the process, use of the initiators in a polymerization process and polymers produced by the polymerization process.

摘要翻译： 制备以下一般结构的单官能胺引发剂的烃溶液的方法：MQnZN（A（R1R2R3））2金属，选自锂，钠和钾，Q是衍生的饱和或不饱和烃基 通过并入选自共轭二烯烃和烯基取代的芳族烃的化合物; Z是含有3-25个碳原子的烃系链基团; A是选自元素周期表IVa的元素，R1，R2和R3独立地选自氢，烷基，取代的烷基，环烷基，芳基或取代的芳基，m是0-7的整数，n是 1至5的整数，通过该方法制备的单官能胺引发剂，在聚合方法中使用引发剂和通过聚合方法制备的聚合物。

公开(公告)号：US5493044A

公开(公告)日：1996-02-20

申请号：US326681

申请日：1994-10-20

申请人： James A. Schwindeman

发明人： James A. Schwindeman

IPC分类号： C07F7/18

CPC分类号： C07F7/188

摘要： A process for preparing alkylsilyl and arylsilyl ethers of the formula(R--O--SiR.sup.1 R.sup.2 R.sup.3)wherein R, R1, R2 and R3 are independently selected from the group consisting of hydrogen, alkyl groups containing one to twenty carbon atoms, substituted alkyl groups containing one to twenty carbon atoms, aryl groups containing six to eighteen carbon atoms, substituted aryl groups containing six to eighteen carbon atoms, hetero aryl groups containing four to eighteen carbon atoms, and substituted hetero aryl groups containing four to eighteen carbon atoms, with the proviso that R is never hydrogen, by reacting, in a hydrocarbon solvent, a chlorosilane of the formula R.sup.1 R.sup.2 R.sup.3 Si--Cl wherein R.sup.1, R.sup.2, and R.sup.3 are independently selected from hydrogen, alkyl groups containing one to twenty carbon atoms, substituted alkyl groups containing one to twenty carbon atoms and aryl groups containing six to eighteen carbon atoms, substituted aryl groups containing six to eighteen carbon atoms, hetero aryl groups containing four to eighteen carbon atoms, and substituted hetero aryl groups containing four to eighteen carbon atoms with an alcohol of the formula ROH wherein R is an alkyl group containing one to twenty carbon atoms, a substituted alkyl group containing one to twenty carbon atoms, an aryl or substituted aryl group containing six to eighteen carbon atoms, or a hetero aryl or substituted hetero aryl group containing four to eighteen carbon atoms, in the presence of an organic acid acceptor (base) in a hydrocarbon solvent.

摘要翻译： 一种制备式（RO-SiR 1 R 2 R 3）的烷基甲硅烷基和芳基甲硅烷基醚的方法，其中R，R 1，R 2和R 3独立地选自氢，含有1-20个碳原子的烷基，含有一至二十个 碳原子数为6〜18个的芳基，6〜18个碳原子的取代芳基，含有4〜18个碳原子的杂芳基，以及含有4〜18个碳原子的取代杂芳基，条件是R为 不得通过在烃溶剂中使式R 1 R 2 R 3 Si-Cl的氯代硅烷反应氢化，其中R 1，R 2和R 3独立地选自氢，含有1-20个碳原子的烷基，含有1-20个碳原子的取代烷基 含有6至18个碳原子的芳基，含有6至18个碳原子的取代芳基，杂芳基 含有4至18个碳原子，和含有4至18个碳原子的取代的杂芳基与式ROH的醇反应，其中R是含有1-20个碳原子的烷基，含1-20个碳原子的取代烷基， 在有机酸受体（碱）存在下，在烃溶剂中，含有6至18个碳原子的芳基或取代的芳基或含有4至18个碳原子的杂芳基或取代的杂芳基。

公开(公告)号：US5403946A

公开(公告)日：1995-04-04

申请号：US279721

申请日：1994-07-25

申请人： James A. Schwindeman

发明人： James A. Schwindeman

IPC分类号： C07F7/18 ,  C07F7/08

CPC分类号： C07F7/1864

摘要： A process for producing compounds of the formula (CH.sub.3).sub.3 SiORLi where in R is selected from alkyl groups containing 2 to 10 carbon atoms and aryl groups containing 6 to 10 carbon atoms by reacting, in an inert atmosphere, in a hydrocarbon solvent, a haloalcohol of the formula HORX wherein R is selected from alkyl groups containing 2 to 10 carbon atoms and aryl groups containing 6 to 10 carbon atoms and X is selected from chlorine or bromine, is reacted with hexamethyldisilazane at a temperature between 20.degree. C. and the reflux temmperature of the solvent after which the resulting product, a trimethylsilyloxyalkylhalide compound, is reacted at a temperature between 50.degree. and 160.degree. C., with powdered lithium metal to produce the (CH.sub.3).sub.3 SiORLi compound.

摘要翻译： 一种制备式（CH3）3SiORLi化合物的方法，其中R选自含有2至10个碳原子的烷基和含6至10个碳原子的芳基，在惰性气氛中，在烃溶剂中，卤代醇 其中R选自含有2至10个碳原子的烷基和含6至10个碳原子的芳基，X选自氯或溴，与六甲基二硅氮烷在20℃和回流温度下反应 溶剂的温度在此之后，所得产物三甲基甲硅烷氧基卤化物化合物在50-160℃的温度下与粉末状锂金属反应，生成（CH3）3SiORLi化合物。

公开(公告)号：US5321148A

公开(公告)日：1994-06-14

申请号：US175833

申请日：1993-12-30

申请人： James A. Schwindeman

发明人： James A. Schwindeman

IPC分类号： C07F7/18 ,  C07F7/08

CPC分类号： C07F7/1892

摘要： A process for preparing functionalized alkyllithium compounds comprising reacting a fine particle size lithium metal of not more than 300 microns average particle size with an organosiloxyalkyl halide of the formula R.sup.1 R.sup.2 R.sup.3 SiORX wherein R.sup.1, R.sup.2 and R.sup.3 are independently selected from alkyl groups containing 1 to 10 carbon atoms and aryl groups containing 6 to 10 carbon atoms, R is selected from alkyl groups containing 1 to 8 carbon atoms either straight chain or substituted by alkyl or aryl groups, X is selected from chlorine or bromine, the reaction temperature is above 50.degree. C., the reaction medium is a hydrocarbon solvent and the reaction is conducted in an inert atmosphere.6-(t-butyldimethylsilyloxy)-1-hexylhalide, 3-(t-butyldimethyl-silyloxy)-2,2-dimethyl-1-propylhalide, 3-(t-butyldimethylsilyloxy)-1-propylhalide, 4-(t-butyldimethylsilyloxy)-1-butylhalide, 3-(t-butyldimethyl-silyloxy)-2-methyl-1-propylhalide 8-(t-butyldimethylsilyloxy)-1-octylhalide, 6-(triisopropylsilyloxy)-1-hexylhalide, 3-(triisopropylsilyloxy)-2,2-dimethyl-1-propylhalide; 3-(triisopropylsilyloxy)-1-propylhalide, 4-(triisopropylsilyloxy)-1-butylhalide, 3-(triisopropylsilyloxy)-2-methyl-1-propylhalide, 8-(triisopropylsilyloxy)-1-octylhalide, 6-(t-butyldiphenylsilyloxy)-1-hexylhalide, 3-(t-butyldiphenylsilyloxy)-2,2-dimethyl-1-propylhalide, 3-(t-butyldiphenylsilyloxy)-1-propylhalide, 4-(t-butyldiphenylsilyloxy)-1-butylhalide, 3-(t-butyldiphenylsilyloxy)-2-methyl-1-propylhalide and 8-(t-butyldiphenylsilyloxy)-1-octylhalide.

摘要翻译： 一种制备官能化烷基锂化合物的方法，包括使平均粒度不超过300微米的细粒度锂金属与式R1R2R3SiORX的有机硅氧烷基卤化物反应，其中R 1，R 2和R 3独立地选自含有1至10个碳原子的烷基 含有6〜10个碳原子的芳基，R选自直链或碳原子数为1〜8的烷基，被烷基或芳基取代，X选自氯或溴，反应温度高于50℃。 反应介质是烃溶剂，反应在惰性气氛中进行。 6-（叔丁基二甲基甲硅烷氧基）-1-己酰卤，3-（叔丁基二甲基甲硅烷氧基）-2,2-二甲基-1-丙基卤，3-（叔丁基二甲基甲硅烷氧基）-1-丙基卤，4-（叔丁基二甲基甲硅烷氧基 ）-1-丁基卤化物，3-（叔丁基二甲基甲硅烷氧基）-2-甲基-1-丙基卤，8-（叔丁基二甲基甲硅烷氧基）-1-辛基卤化物，6-（三异丙基甲硅烷氧基）-1-己基卤化物，3-（三异丙基甲硅烷氧基） -2,2-二甲基-1-丙基卤; 3-（三异丙基甲硅烷氧基）-1-丙基卤，4-（三异丙基甲硅烷氧基）-1-丁基卤，3-（三异丙基甲硅烷氧基）-2-甲基-1-丙基卤，8-（三异丙基甲硅烷氧基）-1-辛酰卤，6-（叔丁基二苯基甲硅烷氧基 ） - 1-己基卤，3-（叔丁基二苯基甲硅烷氧基）-2,2-二甲基-1-丙基卤，3-（叔丁基二苯基甲硅烷氧基）-1-丙基卤，4-（叔丁基二苯基甲硅烷氧基）-1-丁基卤， （叔丁基二苯基甲硅烷氧基）-2-甲基-1-丙基卤和8-（叔丁基二苯基甲硅烷氧基）-1-辛基卤化物。

公开(公告)号：US06699939B2

公开(公告)日：2004-03-02

申请号：US10176723

申请日：2002-06-21

申请人： James A. Schwindeman ,  Robert J. Letchford ,  Conrad W. Kamienski ,  Roderic P. Quirk

发明人： James A. Schwindeman ,  Robert J. Letchford ,  Conrad W. Kamienski ,  Roderic P. Quirk

IPC分类号： C08F29704

CPC分类号： C08F36/04 ,  C08C19/44 ,  C08F4/46 ,  C08F4/48 ,  C08F4/72 ,  C08F8/34 ,  C08F12/04 ,  C08F2810/40 ,  C08F112/08

摘要： Hetero-telechelic polymers having the formula: FG—(Q)d—Z—J—[A(R1R2R3)]x  (I) wherein FG is a protected or non-protected functional group; Q is a saturated or unsaturated hydrocarbyl group derived by incorporation of a compound selected from the group consisting of conjugated diene hydrocarbons, alkenylsubstituted aromatic hydrocarbons, and mixtures thereof; d is an integer from 10 to 200; Z is a branched or straight chain hydrocarbon group which contains 3-25 carbon atoms, optionally containing aryl or substituted aryl groups; J is oxygen, sulfur, or nitrogen; [A(R1R2R3)]x is a protecting group, wherein A is an element selected from Group IVa of the Periodic Table of Elements; R1, R2, and R3 are each independently selected from the group consisting of hydrogen, alkyl, substituted alkyl groups containing lower alkyl, lower alkylthio, and lower dialkylamino groups, aryl or substituted aryl groups containing lower alkyl, lower alkylthio, and lower dialkylamino groups, and cycloalkyl and substituted cycloalkyl containing 5 to 12 carbon atoms; and x is dependent on the valence of J and varies from one when J is oxygen or sulfur to two when J is nitrogen, with the proviso J and FG are not the same, and processes for making the same.

公开(公告)号：US06221991B1

公开(公告)日：2001-04-24

申请号：US09109210

申请日：1998-06-30

申请人： Robert J. Letchford ,  James A. Schwindeman ,  Conrad W. Kamienski ,  Roderic P. Quirk

发明人： Robert J. Letchford ,  James A. Schwindeman ,  Conrad W. Kamienski ,  Roderic P. Quirk

IPC分类号： C08F2054

CPC分类号： C08F20/56 ,  C08F4/46 ,  C08F4/72 ,  C08F8/00 ,  C08F20/14 ,  C08F20/18 ,  C08F20/42 ,  C08F2810/40 ,  C08G81/021 ,  C08F120/14

摘要： Polar polymers having the following formula: FG-(Q)d-Rn-Z-J-[A(R1R2R3)]x   (I) wherein FG is H or a protected or non-protected functional group; Q is a polar hydrocarbyl group derived by incorporation of a polar compound selected from group consisting of esters, amides, and nitrites of acrylic and methacrylic acid, and mixtures thereof; d is an integer from 10 to 2000; R is a saturated or unsaturated hydrocarbyl group derived by incorporation of a compound selected from the group consisting of conjugated diene hydrocarbons, alkenylsubstituted aromatic hydrocarbons, and mixtures thereof; n is an integer from 0 to 5; Z is a branched or straight chain hydrocarbon group which contains 3-25 carbon atoms, optionally containing aryl or substituted aryl groups; J is oxygen, sulfur, or nitrogen; [A(R1R2R3)]x is a protecting group, in which A is an element selected from Group IVa of the Periodic Table of Elements; R1, R2, and R3 are each independently selected from the group consisting of hydrogen, alkyl, substituted alkyl groups containing lower alkyl, lower alkylthio, and lower dialkylamino groups, aryl or substituted aryl groups containing lower alkyl, lower alkylthio, and lower dialkylamino groups, and cycloalkyl and substituted cycloalkyl containing 5 to 12 carbon atoms; and x is dependent on the valence of J and varies from one when J is oxygen or sulfur to two when J is nitrogen, and living anionic polymerization processes for preparing the same.

摘要翻译： 具有下式的极性聚合物：其中FG是H或被保护或未被保护的官能团; Q是通过掺入选自丙烯酸和甲基丙烯酸的酯，酰胺和亚硝酸盐的极性化合物及其混合物衍生的极性烃基; d为10〜2000的整数， R是通过引入选自共轭二烯烃，烯基取代的芳族烃及其混合物的化合物衍生的饱和或不饱和烃基; n为0〜5的整数， Z是含有3-25个碳原子的支链或直链烃基，任选含有芳基或取代的芳基; J是氧，硫或氮; [A（R 1 R 2 R 3）] x是保护基，其中A是选自元素周期表Ⅳa族的元素; R 1，R 2和R 3各自独立地选自氢，烷基，含有低级烷基，低级烷硫基和低级二烷基氨基的取代烷基，含有低级烷基，低级烷硫基和低级二烷基氨基的芳基或取代芳基 和含有5至12个碳原子的环烷基和取代的环烷基; 并且x取决于J的化合价，并且当J为氮时J为氧或硫时为2，并且当用于制备其的活性阴离子聚合方法时，其为不同的。

公开(公告)号：US06184309B2

公开(公告)日：2001-02-06

申请号：US09207226

申请日：1998-12-08

申请人： James A. Schwindeman ,  John F. Engel ,  Eric J. Granger ,  Conrad W. Kamienski ,  Roderic P. Quirk

发明人： James A. Schwindeman ,  John F. Engel ,  Eric J. Granger ,  Conrad W. Kamienski ,  Roderic P. Quirk

IPC分类号： C08F800

CPC分类号： C08C19/00 ,  C08F8/00 ,  C08F2810/40 ,  C08F112/08 ,  C08F120/14

摘要： A process for removing a protecting group from a polymer. Protected functional groups of a polymer may be deprotected by treating the polymer in the presence of an acid catalyst, including organic acids, mineral acids, heterogeneous acid systems, Lewis acids, and fluoride ion sources.

摘要翻译： 从聚合物中除去保护基团的方法。 通过在酸催化剂存在下处理聚合物，包括有机酸，无机酸，多相酸体系，路易斯酸和氟离子源，可以将保护的聚合物的官能团脱保护。

公开(公告)号：US6060617A

公开(公告)日：2000-05-09

申请号：US670348

申请日：1996-06-25

申请人： Randy W. Hall ,  Bobby J. McElroy ,  James A. Schwindeman ,  Conrad W. Kamienski ,  Terry L. Rathman ,  Robert C. Morrison

发明人： Randy W. Hall ,  Bobby J. McElroy ,  James A. Schwindeman ,  Conrad W. Kamienski ,  Terry L. Rathman ,  Robert C. Morrison

IPC分类号： C07C211/65 ,  C07F7/10

CPC分类号： C07F7/10 ,  C07C211/65

摘要： Organometallic amide compositions and processes for preparing the same, for example, by: reacting an alkali metal, alkali metal hydride, or alkali metal amide with a substituted amine in the absence of an electron carrier; reacting an alkali metal with a substituted amine in the presence of an electron carrier in a hydrocarbon solvent; distilling a composition which includes an alkali metal amide and a reduced electron carrier to recover the alkali metal amide; reacting an alkali metal with a substituted amine in the presence of an alkyl halide; and reacting a substituted amine capable of reacting with an alkali metal to form a hydrocarbon insoluble alkali metal amide with an alkali metal in the presence of a substituted amine capable of reacting with an alkali metal to form a hydrocarbon soluble alkali metal amide.

摘要翻译： 有机金属酰胺组合物及其制备方法，例如：在不存在电子载体的情况下使碱金属，碱金属氢化物或碱金属氨化物与取代的胺反应; 在电子载体存在下在烃溶剂中使碱金属与取代的胺反应; 蒸馏包含碱金属氨化物和还原电子载体以回收碱金属胺的组合物; 在烷基卤存在下使碱金属与取代的胺反应; 并使能够与碱金属反应的取代的胺与能够与碱金属反应形成烃溶性碱金属氨化物的取代胺存在下与碱金属形成不溶于烃的碱金属胺。

公开(公告)号：US5976403A

公开(公告)日：1999-11-02

申请号：US65782

申请日：1998-04-23

申请人： B. Troy Dover ,  Conrad W. Kamienski ,  Robert C. Morrison ,  R. Thomas Currin, Jr. ,  James A. Schwindeman

发明人： B. Troy Dover ,  Conrad W. Kamienski ,  Robert C. Morrison ,  R. Thomas Currin, Jr. ,  James A. Schwindeman

IPC分类号： B01J13/00 ,  B22F1/00 ,  B22F9/06 ,  C01D7/00 ,  C01D15/08 ,  C09K3/00 ,  C07C31/30 ,  C07F1/02 ,  C07F1/04

CPC分类号： C01D7/00 ,  B01J13/0086 ,  B22F1/0088 ,  B22F9/06 ,  C01D15/08 ,  Y10S516/926 ,  Y10S516/928 ,  Y10T428/2991

摘要： A process for producing dispersions of atmospherically stable, coated alkali metal particles and atmospherically stable, coated alkali metal powders by agitating a mixture of molten alkali metal in a hydrocarbon oil at dispersion speeds, optionally in the presence of a dispersing agent, contacting the molten alkali metal-hydrocarbon oil dispersion, above or below the surface of the dispersion, with up to 3 weight percent anhydrous carbon dioxide while agitating the dispersion for at least 1 minute. The dispersion in oil can be used directly in chemical reactions. The bulk of the oil can be removed from the dispersions to produce oil wet particles, the oil wet particles car be washed with a low boiling hydrocarbon to produce hydrocarbon wet particles which can be dried to produce atmospherically stable powders of coated metal particles. The dispersed particles in oil, the oil wet particles, the hydrocarbon wet particles and the atmospherically stable powders can each be used in chemical reactions. After washing and drying, the process produces lithium powders having a surface coating composition containing 0.1-0.3 atom percent lithium, 0.3-0.4 atom percent carbon, and 0.3-0.5 atom percent oxygen. The products of the invention may be used to synthesize organometallic compounds, esp. n-butyl lithium and sec-butyl lithium, having low color and low soluble inorganic chloride levels.

摘要翻译： 通过搅拌熔融碱金属在烃油中的分散速度的混合物，任选地在分散剂存在下，使熔融碱接触，制备大气稳定的涂覆的碱金属颗粒和大气稳定的包覆的碱金属粉末的分散体的方法 在分散体表面上方或下方的金属 - 烃油分散体与最多3重量％的无水二氧化碳同时搅拌分散体至少1分钟。 油中的分散体可以直接用于化学反应。 大部分油可以从分散体中除去以产生油湿颗粒，用低沸点烃洗涤油湿颗粒汽车以产生烃湿颗粒，其可以被干燥以产生大气稳定的涂覆金属颗粒的粉末。 油中的分散颗粒，油湿颗粒，烃湿颗粒和气氛稳定的粉末均可用于化学反应。 洗涤和干燥后，该方法产生具有表面涂层组合物的锂粉末，其中含有0.1-0.3％原子百分比的锂，0.3-0.4％的碳和0.3-0.5％的氧。 本发明的产品可用于合成有机金属化合物， 正丁基锂和仲丁基锂，颜色低，可溶性无机氯化物水平低。

公开(公告)号：US5912378A

公开(公告)日：1999-06-15

申请号：US851324

申请日：1997-05-05

申请人： James A. Schwindeman

发明人： James A. Schwindeman

IPC分类号： C07F7/18 ,  C07F7/08

CPC分类号： C07F7/1864

摘要： A process for producing compounds of the formula (CH.sub.3).sub.3 SiORLi, wherein R is selected from alkyl groups containing 2 to 10 carbon atoms and aryl groups containing 6 to 10 carbon atoms, by reacting, optionally in the presence of a catalyst, in an inert atmosphere, a haloalcohol of the formula HORX, wherein R is selected from alkyl groups containing 2 to 10 carbon atoms and aryl groups containing 6 to 10 carbon atoms and X is selected from chlorine or bromine, is reacted with neat hexamethyldisilazane at a temperature between 20.degree. C. and 200.degree. C., optionally in the presence of a catalyst, after which the resulting product, a trimethylsilyloxyalkylhalide compound, is reacted at a temperature between 50.degree. C. and 160.degree. C., with powdered lithium metal, in an inert hydrocarbon medium, to produce the (CH.sub.3).sub.3 SiORLi compound.

摘要翻译： 一种制备式（CH3）3SiORLi化合物的方法，其中R选自含2至10个碳原子的烷基和含6至10个碳原子的芳基，任选在催化剂存在下，在惰性 气氛中，式（Ⅳ）的卤代醇，其中R选自含有2至10个碳原子的烷基和含6至10个碳原子的芳基，X选自氯或溴，与纯六甲基二硅氮烷在20℃ ℃和200℃，任选地在催化剂存在下，然后将所得产物三甲基甲硅烷氧基烷基卤化合物在50℃至160℃的温度下与粉末状锂金属反应， 惰性烃介质，生成（CH3）3SiORLi化合物。