序号 专利名 申请号 申请日 公开(公告)号 公开(公告)日 发明人
141 Stereoselective preparation and their use of the Grignard compound JP2000559157 1999-07-02 JP2002520339A 2002-07-09 カイエス,ジェラルド; ノッチェル,ポール; ボイモンド,ローレ; ロットランデール,マリオ
(57)【要約】 本発明は、式(I)のグリニャール化合物の立体選択的製造方法、式(Ia)のポリマー結合化合物、物質のライブラリーを作製するための該方法の使用、ならびに立体選択的化学合成における式(I)および(Ia)の化合物の使用に関する。
142 (R *, r *) - 2 - [(dimethylamino) methyl] -1- (3-methoxyphenyl) improved synthesis and purification of cyclohexanol hydrochloride JP2000550815 1999-05-20 JP2002516302A 2002-06-04 エサ・ティ・ジャービ; ニール・エイ・グレイソン; ロバート・イー・ハルバックス
(57)【要約】 (R * ,R * )-2-[(ジメチルアミノ)メチル]-1-(3-メトキシフェニル)シクロヘキサノール(トラマドール)を、該添加剤を使用せずに得られる場合より生成物のトランス:シス比が高度となる該添加剤の存在下でのグルニャール反応で合成する。 アミンまたはエーテル添加剤の存在下での、3-ブロモアニソールおよび適切なマンニッヒ塩基間のグリニャール反応により、トランス/シス割合が改善されたアミン生成物が得られる。 この塩基をその塩酸塩に変換し、アセトニトリルなどの低分子量ニトリル溶媒から、98%以上のトランス/シス割合が得られるまで再結晶する。 イソプロパノールからの再結晶で、ニトリル溶媒を含まない(R * ,R * )-2-[(ジメチルアミノ)メチル]-1-(3-メトキシフェニル)シクロヘキサノール塩酸塩が得られる。 トルエンの存在下でHClをトラマドール塩基に加える工程を含めることにより、トランス:シスの割合を増加させずに、トラマドール塩酸塩を合成することができる。
143 Production of (3-alkoxyphenyl)magnesium chloride and its usage JP3083397 1997-02-14 JPH09227575A 1997-09-02 MITSUHIYAERU FUINKAMU; TOMAASU KOONEN; UERUNAA UINTAA
PROBLEM TO BE SOLVED: To provide a method for producing a (3-alkoxyphenyl)magnesium chloride, and to provide a method for using this compound in the reaction of a specific carbonyl compound. SOLUTION: This (3-C 1-5alkoxyphenyl)magnesium chloride is obtained by reaction of the corresponding (3-alkoxyphenyl) chloride with an activated magnesium prepared by reducing a magnesium halide by an alkali metal. COPYRIGHT: (C)1997,JPO
144 IMPROVED PROCESS FOR PREPARING O-CHLOROMETHYLPHENYLGLYOXYLIC ESTERS, IMPROVED PROCESS FOR PREPARING (E)-2-(2-CHLOROMETHYLPHENYL)-2-ALKOXIMINOACETIC ESTERS, AND NOVEL INTERMEDIATES FOR THEIR PREPARATION PCT/EP2008054354 2008-04-10 WO2008125592B1 2008-12-24 WIEGAND JOHN-MATTHIAS; LUETTGEN KARSTEN; SKRANC WOLFGANG
An improved process for preparing o-chloromethylphenylglyoxylic esters of the formula (I) which comprises converting a compound of the formula (II) by reaction with magnesium into the corresponding Grignard reagent which is then reacted with a compound of the formula (III) to give the compound of the formula (IV) which is then cleaved by reaction with a chloroformic ester of the formula ClCOOR4 or by reaction with phosgene to give the compound of the formula (I), followed by the isolation of the compound of the formula (I), and also an improved process for preparing (E)-2-(2-chloromethylphenyl)- 2-alkoximinoacetic esters of the formula (VII) and intermediates for their preparation.
145 GRIGNARD REACTIONS IN MICROREACTORS PCT/EP2007006127 2007-07-11 WO2008009378A3 2008-03-20 ROBERGE DOMINIQUE; BIELER NIKOLAUS; DUCRY LAURENT
The present invention relates to a process for Grignard type reactions comprising mixing at least two fluids in a microreactor having at least two injection points.
146 Preparation and use of magnesium amides EP11166878.6 2007-01-18 EP2360161B1 2016-08-31 Knochel, Paul; Krasovskiy, Arkady; Krasovskaya, Valeria; Rohbogner, Christoph, Josef; Clososki, Gliuliano, Cesar
147 Organometallic reaction method EP02738825.5 2002-06-27 EP1405840B1 2014-08-20 KIN, Idan; OHTA, Genichi; TERAISHI, Kazuo; WATANABE, Kiyoshi
148 PROCESS FOR PRODUCTION OF BIPHENYL DERIVATIVES EP06822282.7 2006-10-25 EP1955990B1 2012-08-22 HAYASHI, Tamio; NAKATANI, Jiro
A process for the production of biphenyl derivatives represented by the general formula (1), which is characterized by comprising reacting the chlorine atom of a benzene derivative represented by the general formula (2) with metallic magnesium to form a Grignard reagent and coupling two molecules of the Grignard reagent with each other in the presence of a catalyst and which is excellent in industrial productivity by virtue of its using inexpensive and easily available raw materials. (1) (2) (wherein A’s are at least one member selected from between trifluoromethyl and fluoro; and n is an integer of 1 to 4)
149 Process for producing cycloalkyl alkyl ethers EP10189460.8 2002-06-27 EP2279995A2 2011-02-02 Kin, Idan; Ohta, Genichi; Teraishi, Kazuo; Watanabe, Kiyoshi

The invention consists in a process for producing a cycloalkyl alkyl ether compound of formula (1): R1-O-R2, wherein R1 represents a cyclopentyl group or cyclohexyl group which may have a substituent and R2 represents an alkyl group having 1 to 10 carbon atoms or a cycloalkyl group having 3 to 8 carbon atoms which may have a substituent; said process comprising reacting an alicyclic olefin with an alcohol in the presence of an acidic ion-exchange resin having a water content of 5 wt.-% or less. Preferably, the process comprises reacting a gaseous alicyclic olefin with a gaseous alcohol in the presence of an acidic ion-exchange resin having a water content of 5 wt.-% or less.

150 Grignard reactions in microreactors EP09011852.2 2007-07-11 EP2138500A1 2009-12-30 Bieler, Nikolaus; Ducry, Laurent; Roberge, Dominique

The present invention relates to a process for Grignard type reactions comprising mixing at least two fluids in a microreactor having at least two injection points.

151 UNIVERSAL GRIGNARD METATHESIS POLYMERIZATION EP07814646.1 2007-08-31 EP2061825A1 2009-05-27 MCCULLOUGH, Richard, D.; IOVU, Mihaela, C.; OSAKA, Itaru
Universal Grignard Metathesis (GRIM) reactions which provide access to conjugated polymers by GRTM methods are disclosed. Furthermore revealed is a method comprising: providing an unsaturated ring compound comprising at least two halogen ring substituents, providing an organomagnesium reagent comprising an organomagnesium component and a metal activation agent, combining the unsaturated ring compound with the reagent to form a second compound by metal-halogen exchange, wherein the metal activation agent activates the metal-halogen exchange, coupling the second compound to itself in an oligomerization or polymerization reaction. Metal activation agent can be lithium chloride. The process is commercially attractive and can be executed in good yields. Polyfluorenes, polypyrroles, and polythiophenes can be prepared for use in OLED, PLED, photovoltaic, transistor, antistatic coatings, and sensor applications.
152 Process for the production of tertiary alcohols EP07013809.4 2007-07-13 EP2014633A1 2009-01-14 McGarrity, John; Djojo, Francis

Tertiary alcohols are prepared by reacting carboxylic esters with Grignard reagents in ethereal solvents in the presence of lanthanum trichloride and lithium chloride.

The method is particularly suitable for the production of (αS)-α-[3-[(1E)-2-(7-chloro-2-quinolinyl)ethenyl]phenyl]-2-(1-hydroxy-1-methylethyl)benzenepropanol of formula which is an intermediate in the production of montelukast.

153 Preparation and use of magnesium amides EP06001017.0 2006-01-18 EP1810974A1 2007-07-25 Knochel, Paul; Krasovskaya, Valeria; Krasovskiy, Arkady

The present application relates to mixed Mg/Li amides of the general formula



         R1R2N-MgX·zLiY     (I),



wherein

R1, R2 and R3 independently are selected from substituted or unsubstituted aryl or heteroaryl containing one or more heteroatoms, linear, branched or cyclic, substituted or unsubstituted alkyl, alkenyl, alkynyl, or derivatives thereof, and, for R1 and R2 only, the silyl derivatives thereof; one of R1 and R2 may be H; or R1 and R2 together can be part of a cyclic or polymeric structure;

X and Y independently are selected amongst others from the group consisting of F; Cl; Br; I; CN; SCN; NCO; and z > 0, as well as a process for the preparation of the mixed Mg/Li amides and the use of these amides, e.g. as bases.

154 SOLVENTS CONTAINING CYCLOALKYL ALKYL ETHERS AND PROCESS FOR PRODUCTION OF THE ETHERS EP02738825 2002-06-27 EP1405840A4 2006-05-17 KIN IDAN; OHTA GENICHI; TERAISHI KAZUO; WATANABE KIYOSHI
A solvent containing at least one cycloalkyl alkyl ether (1) represented by the general formula: R1-O-R2 (wherein R1 is cyclopentyl or the like; and R2 is C1-10 alkyl or the like); and a process for the production of the ethers (1), characterized by reacting an alicyclic olefin with an alcohol in the presence of an acid ion-exchange resin having a water content of 5 wt% or below. The solvent is useful as cleaning solvent for electronic components, precision machinery components or the like, reaction solvent for various chemical reactions, extraction solvent for extracting objective organic substances, solvent or remover for electronic and electrical materials, and so on. The process enables industrially advantageous production of the objective cycloalkyl alkyl ethers (1).
155 Process for preparing unsymmetrical biaryls and alkylated aromatic compounds from arylnitriles EP02102055.7 2002-07-25 EP1279656A3 2004-10-06 MILLER, Joseph A.

Methods are provided for the construction of unsymmetrical biaryl compounds and alkylated aromatic compounds from arylnitriles using a nickel or palladium catalyzed coupling in which the catalyst has at least one phosphorus ligand.

156 AN IMPROVED SYNTHESIS AND PURIFICATION OF (R*,R*)-2- (DIMETHYLAMINO) METHYL]-1-( 3-METHOXYPHENYL) CYCLOHEXANOL HYDROCHLORIDE EP99930115.3 1999-05-20 EP1077923B1 2004-01-02 JARVI, Esa, T.; GRAYSON, Neile, A.; HALVACHS, Robert, E.
(R*,R*)-2-[ (dimethylamino) methyl]-1-( 3-methoxyphenyl) cyclohexanol (Tramadol) is synthesized in a Grignard reaction in the presence of an additive resulting in a higher trans:cis ratio of product than is obtained in the absence of the additive. The Grignard reaction between 3 bromoanisole and the appropriate Mannich base in the presence of an amine or ether additive gives the amine product in an improved trans/cis ratio. The base is converted to its hydrochloride and recrystallized from a low molecular weight nitrile such as acetonitrile until a greater than 98 % trans/cis ratio is obtained. Recrystallization from isopropanol gives (R*,R*)-2-[(dimethylamino)methyl]-1-(3-methoxyphenyl)cyclohexanol hydrochloride free of the nitrile solvent. A hydrochloride of Tramadol can be synthesized without increasing a ratio of trans:cis by including a step in which HCl is added to Tramadol base in the presence of toluene.
157 A microreactor EP03250834.3 2003-02-11 EP1336431A2 2003-08-20 Gilligan, Mark Peter Timothy; Homewood, Philip James; Whiffin, Rowland

A microreactor with a sensor 9, 11 in a reaction channel 6. The sensor comprises a pair of spaced apart electrodes through which an AC voltage is passed. The amplitude and phase of the current flowing between the electrodes is monitored allowing the impedance of the reaction fluid between the electrodes to be measured.

158 FLUOROUS PHOSPHINES AND PROCESS FOR THEIR PREPARATION EP99949444.6 1999-09-29 EP1117668B1 2002-12-11 RICHTER, Bodo; DE WOLF, Aloysius, Cornelius, Adrianus; VAN KOTEN, Gerard; DEELMAN, Berth, Jan
A fluorous phosphine wherein the phosphor is coupled to at least one aryl or alkyl moiety, to which moiety a fluorous tail is coupled, wherein a spacer group, containing a non-carbon atom, is positioned between the aryl or alkyl moiety and the fluorous tail, a process for the preparation of said phosphines, metalcomplexes, catalysts and catalyst compounds therefrom and their use in catalysis.
159 Herstellung und Verwendung von (3-Alkoxyphenyl)magnesiumchloriden EP97101270.3 1997-01-28 EP0790251B1 2002-12-04 Finkam, Michael, Dr.; Kohnen, Thomas; Winter, Werner, Prof. Dr.
160 REAKTION VON CARBONYLVERBINDUNGEN MIT METALLORGANISCHEN REAGENZIEN EP01900150.2 2001-01-10 EP1246784A1 2002-10-09 KOOP, Ulrich; KRUMMRADT, Holger; SCHWARZ, Michael; STOLDT, Jöran; ECKSTEIN, Jürgen; ZEHNER, Stefan; MELICHAR, Wolfgang
The invention relates to a novel method for carrying out reactions of carbonyl compounds with organometallic reagents, especially grignard reagents. The inventive method is characterised in that the organometallic reagent and the carbonyl compound are provided and tempered separately in a suitable solvent before being pumped into a tempered mini/micromixer.
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