A method for production of alkyl(phenyl)phosphine complexes baranovich
(57) Abstract:
The invention relates to the chemistry of organophosphorus compounds with s-R connection, namely to obtain alkyl(phenyl)phosphine-Baranovka complex of the General formula R2PHBH3(1), where R is alkyl or phenyl, which are used as starting substances for the synthesis of water-soluble catalysts used in the production of polymers. Describes how to obtain alkyl(phenyl)phosphine-Baranovka complex interaction dialkyl(diphenyl)chlorophosphines with a complex hydride with sodium borohydride in an organic solvent is dimethyl ether of ethylene glycol, at a temperature of 10-100oWith original reagents taken in equimolar ratio with subsequent isolation of the target product known techniques. The technical result is a significant simplification and cheapening of the process and however obtaining a high quality product with a high yield of 70-90% and the content of the main substance of 95%. 2 C.p. f-crystals. The present invention relates to the chemistry of organophosphorus compounds with C-R-communication, namely to obtain alkyl(phenyl)phosphine-Baranovich complexes of General formulaR2MVN3(1),
R - Ala is used in the production of polymers.A method of obtaining alkyl(phenyl)phosphine-Baranovich complexes of the General formula (1) interaction dialkyl(diphenyl)chlorophosphines with lithium aluminum hydride and borane in tetrahydrofuran, the original reactants are taken in equimolar ratio, followed by separation of the target product by extraction with benzene, selected as a prototype (J. Am. Chem. Soc., 1990, 112, 5244-5252).The disadvantage of the prototype is the use of volatile borane and explosive and quite expensive lithium aluminum hydride.Task to be solved by the present invention is directed, is simpler and cheaper method of producing alkyl(phenyl)phosphine-Baranovich complexes.This problem is solved by that in a method of producing alkyl(phenyl)phosphine-Baranovich complexes of the General formula (1) interaction dialkyl(diphenyl)chlorophosphines with a complex hydride in the environment of an organic solvent at equimolar ratio of the initial reagents, followed by separation of the target product, according to the invention as a complex hydride use borohydride sodium, as the organic solvent is dimethyl ether of ethylene glycol and the reaction is conducted at a temperature of 10-100


BAS-L-Bc-L'-(Bc'-L")n-BAS',
where BAS, BAS', BAS"- bioactive ingredients, which may be identical or different; Su and Su' - complexes phenylboric acid; L, L', L" - linkers; n = 0 or 1, three methods for their production, intermediate products used in their synthesis and representing phenylboronic complexing reagents and phenylboronic cross-linking reagents, the method of selection of the desired cell population, as well as set or system containing bioconjugate And, to scroll to the desired population of cells

m is 0 or 1;
p is 0;
X represents oxygen or sulfur;
Y represents CH, N or NO;
W represents oxygen or H2;
And represents N or C(R2);
G represents N or C(R3);
D represents N or C(R4)
provided that not more than one of A, G and D represents nitrogen, but at least one of Y, a, G, and D represents nitrogen or NO;
R1represents hydrogen or C1-C4-alkyl;
R2, R3and R4are independently hydrogen, halogen, C1-C4-alkyl, C2-C4alkenyl,2-C4-quinil, aryl, heteroaryl, including five - or six-membered aromatic ring with 1 or 2 nitrogen atoms, as well as furyl or morpholyl, HE OS1-C4-alkyl, CO2R1, -CN, -NO2, -NR5R6or R2and R3or R3and R4accordingly, together with part a and G or G and D southwest a hydrogen, WITH1-C4-alkyl, C(O)R7C(O)OTHER8WITH(O)OR9, SO2R10, -NR5R6, (CH3)3Si and phenyl, or may together represent (CH2)jQ(CH2)kwhere Q represents a bond; j is 2 and k is 0 to 2;
R7, R8, R9, R10and R11are independently C1-C4-alkyl, NH2, aryl or its enantiomer,
and their pharmaceutically acceptable salts, and methods for their preparation, intermediate compounds and pharmaceutical compositions, which has an activating effect against nicotine


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FIELD: chemistry of organometallic compounds.
SUBSTANCE: invention relates to a method for preparing lithium complexes salts of the general formula (I): wherein each radical R3-R6 means hydrogen atom (H) or halogen atom (F, Cl or Br). Method involves mixing a) 3-, 4-, 5-, 6-substituted phenol of the formula (III):
wherein R3-R6 have above given values with chlorosulfonic acid in acceptable solvent to yield compound of the formula (IV):
; b) intermediate product of the formula (IV) from the stage a) wherein R3-R6 have values given above is subjected for interaction with chlorotrimethylsilane to yield compound of the formula (II) given in the invention description and obtained product is filtered off and subjected for differential distillation; c) intermediate product (II) from the stage b) is subjected for interaction with tetramethanolate borate lithium (1-) in acceptable solvent and the end product (I) is isolated from it. Invention provides the development of a simple method for synthesis of lithium complex salts.
EFFECT: improved preparing method.
3 cl, 4 ex
FIELD: polymerization catalysts.
SUBSTANCE: invention relates to novel organometallic compounds and to olefin polymerization catalytic systems including such organometallic compounds, and also to a method for polymerization of olefins conduct in presence of said catalytic system. Novel organometallic compound is prepared by bringing into contact (i) compound of general formula I: (I), where Ra, Rb, Rc, and Rd, identical or different, represent hydrocarbon groups; and (ii) Lewis acid of general formula MtR
EFFECT: enabled preparation of novel olefin polymerization cocatalysts, which reduce use of excess cocatalyst relative to alkylalumoxanes, do not lead to undesired by-products after activation of metallocene, and form stable catalytic compositions.
14 cl, 1 tbl, 32 ex
FIELD: chemistry of organophosphorus compounds.
SUBSTANCE: invention relates to compounds with the bond C-P, namely to phosphorus-boron-containing methacrylate that can be used as inhibitor of combustion of polyvinyl alcohol-base film materials. Invention describes phosphorus-boron-containing methacrylate of the following formula: wherein n = 4-8. Polyvinyl alcohol films modified with indicated phosphorus-boron-containing methacrylate shows the enhanced refractoriness, rupture strength up to 206 kgf/cm2, water absorption up to 240% and relative elongation up to 12%.
EFFECT: valuable properties of substance.
1 tbl, 2 ex
FIELD: chemistry of complex compounds.
SUBSTANCE: invention relates to new derivatives of boranocarbonate of the formula (I): wherein X1 means -H; X3 and X2 mean similar or different substitutes that are taken among the group consisting of -H, -NHxRy at x + y = 3, or -R wherein R means substitute that is bound with nitrogen or boron atom through carbon atom, respectively, and represents methyl or ethyl group; Y means group -OH, -OH2, -OR or -NHR wherein R means substitute that is bound with nitrogen or oxygen atom through carbon atom, respectively, and represents methyl or ethyl group; or their salts. Invention provides using prepared compounds as source of carbon monoxide (CO) and as a reducing agent in preparing carbonyl metal complexes in an aqueous solution. Also, invention involves a method for preparing borane carbonate and a method for reducing with using H3BCO as a reducing agent.
EFFECT: improved method for preparing.
20 cl, 14 ex
FIELD: organic synthesis.
SUBSTANCE: invention relates to organoboron compounds technology, in particular to aminoboranes and, more specifically, to trimethylaminoborane, which can be used as reducing and hydroboronizing agents as well as in color photography, in magnetic film manufacture, and as fuel additive to decrease amount of deposits in combustion chamber. Method comprises reaction of trimethylamine with gaseous diborane in organic solvent at reduced temperature. Solvent is selected from aliphatic, cycloaliphatic, and aromatic hydrocarbons with melting temperature not higher than -20°C. Reaction is conducted at temperature from -30°C to 0°C, preferably from -15 to -5°C, at trimethylamine-to-solvent volume ratio 1:(1/5-3.5).Proposed method simplifies preparation procedure owing to eliminated laborious solvent removing vacuum distillation stage and stage wherein of aqueous alkali metal hydroxide is introduced to stabilize aminoborane. Yield of desired product, characterized by high purity, achieves 95-98.6%, which is essentially higher than, for example yield (86%) of morpholinoborane regarded as prototype compound in a known process.
EFFECT: enhanced economical efficiency of process.
3 cl, 4 ex
FIELD: chemical technology.
SUBSTANCE: invention relates to technology for preparing organoboron compounds, in particular, to the improved method for preparing 9-borabicyclo[3.3.1]nonane. Method for preparing 9-borabicyclo[3.3.1]nonane is carried out by interaction of diborane with 1,5-cyclooctadiene in 1,4-dioxane medium at simultaneous feeding diborane and 1,5-cyclooctadiene at the rate necessary for maintaining the molar ratio 1,5-cyclooctadiene : diborane = (1.9-2.04):1.0, respectively, during all through reaction. The process is carried out in the volume ratio 1,4-dioxane : 1,5-cyclooctadiene = (2.2-4.0):1.0 and at temperature 11-25°C. In preparing 9-borabicyclo[3.3.1]nonane the reaction mass is kept at temperature 65-102°C. The invention provides simplifying technology in preparing 9-borabicyclo[3.3.1]nonane due to exclusion the preliminary preparing borane complex and additional recrystallization of 9-borabicyclo[3.3.1]nonane, enhancing yield of the end product up to 91.0-93.5% of the high quality (the content of basic substance is 99.1-99.9%, melting point is 152-156°C), and possibility for creating the wasteless manufacturing. Method for preparing 9-borabicyclo[3.3.1]nonane shows technological simplicity in its realization and economy profit in its realization in industrial scale.
EFFECT: improved preparing method.
4 cl, 4 ex