51 results about "BINAP" patented technology

The invention discloses applications of a chiral polymer catalyst in asymmetric reaction, and belongs to the field of material synthesis and application. The phosphine-containing polymer is obtained via mixed polymerization of vinyl-containing chiral bidentate phosphine ligand BINAP (2,2'-bis(diphenylphosphino)-1,1'-binaphthyl) and derivative of vinyl-containing chiral bidentate phosphine ligand BINAP (2,2'-bis(diphenylphosphino)-1,1'-binaphthyl) with other vinyl comonomers. The vinyl polymer possesses relatively large specific surface area and porosity, and excellent thermal stability and chemical stability. In the heterogeneous catalyst, one or a plurality of elements selected from Ru, Rh, Ir, Pa, Au, and Cu are taken as active ingredients. The chiral ligand is uniformly embedded into and highly dispersed in a polymer skeleton, so that metal dispersion degree on the catalyst is relatively high, and relatively high catalytic activity is achieved. The heterogeneous catalyst is suitable for a plurality of reaction technology including intermittent still reaction, continuous fixed bed reaction, and trickle bed reaction. When the heterogeneous catalyst is used in catalytic kettle-type asymmetric hydrogenation, high target product yield is achieved, and enantioselectivity is higher than 96%.

The invention discloses an optically-active helix chain poly(phenyl isocyanide) and a polymerization method thereof. The polymerization process is shown as the general formula in the description; in the formula, the structural formula of a chiral phosphine ligand is shown in the description. A palladium catalyst is adopted, the chiral phosphine ligand (S-or R-BINAP) is added to induce polymerization of achiral phenyl isocyanide, and the optically-active polymer with excessive one-handed helixes is obtained; obtained poly(phenyl isocyanide) has a high molecular weight and narrow molecular weight distribution.

The invention relates to a synthesis method of polyuralcohol, belonging to polymer technical field, which comprises that adds dihalide aromatic ketone, sodium tert-butoxide NaOt-Bu, 1, 1'-dinaphthalene-2, 2'-diphenylphosphino BINAP, aromatic diamine and Pd2(dba)3 into a three-mouth flask with nitrogen gas feeding in turn, wherein the mole ratio is 1:1:2.8:0.03:0.01, adds N, N-dimethylacetamide until the monomer density is 0.5-0.65mol / L, increases temperature from 20DEG C to 100DEG C, keeps for 4-6h, increases temperature from 100DEG C to 150-200DEG C, keeps for 20-24h, cools to 20DEG C, adds the mixture of ammonia and methanol at the ratio of 1:4(L / L), mixes, stands for 1h, washes via the mixture of ammonia and methanol for three times, filters, dries at vacuum for 6h, mixes and dissolves poly(imino ketone) and benzoyl chloride in tetrahydrofuran for 2-12h at 1-3DEG C, to obtain polyuralcohol to be dried. The synthesized polyuralcohol Tg is higher than 190DEG C and TD is higher than 450DEG C, with better heat stability and dynamic mechanical stability.

The invention provides a heterogeneous catalyst for Beta-ketoesters and application thereof and belongs to the field of material synthesis and catalyst application.The catalyst comprises a metal component and a carrier.A preparation method of the catalyst carrier comprises: subjecting commonly used chiral ligand BINAP(2,2'-bis(diphenylphosphine)-1,1'-binaphthyl) not modified to Friedel-Crafts reaction, copolymerizing with other monomers such as benzene through L-acid catalysis by using dimethoxymethane as a cross-linking agent, acquiring a chiral hyper-cross-linked material of various ducts, mainly micropores, through a one-step method.The metal component uses Ru2(C6H6)2Cl4 as a metal precursor.By using the catalyst provided herein in asymmetric hydrogenation of methyl acetoacetate under 2-6 Mpa at 20-100 DEG C, it is possible to acquire high-activity and about 95% of enantio-selectivity in methanol solution, and more than six times of reuse are available.

The invention discloses a synthetic method of 2,2'-double diphenyl phosphine-1,1'-dinaphthalene. The method comprises the following steps: adding a lithium metal sheet, a ligand, 2,2'-diethoxy-1,1'-dinaphthalene and an ethers solvent are added in a reaction still, heating the materials to the temperature of 60-140 DEG C, reacting the materials for 6-12 hours, dropping chlorodiphenylphosphine at the temperature of 0 DEG C, heating the material to room temperature, and obtaining the product after the reaction is completed; equivalent water quenching is carried out, a product solution is concentrated and filtered, a filter cake is washed with methanol, and vacuum drying is carried out to obtain the product 2,2'-double diphenyl phosphine-1,1'-dinaphthalene (BINAP). The method has the advantages of high yield, low preparation cost, simple post-treatment, high product purity, and is suitable for process enlargement.

The invention discloses a synthesis method of (R)-5'-methoxyl laudanosine, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: by taking 6,7-dimethoxy-1-(3,4,5-trimethoxybenzyl)-3,4-dihydroisoquinoline as a raw material, sequentially carrying out N-formylation, asymmetric hydrogenation reduction and formyl reduction to obtain (R)-5'-methoxy laudanosine. According to the technical scheme, the yield of (R)-5'-methoxyl laudanosine directly prepared is high, the total yield of the three-step reaction can reach up to 81.9%, the optical purity is 99.79% or above, and after refining, the optical purity is larger than 99.98%, and the chemical purity is larger than 99.93%. Besides, according to the technical scheme, the chiral selective catalyst Ru(CH3COO)2(R)-BINAP without genotoxicity is adopted, the defect that genotoxic impurities containing p-toluenesulfonyl and the like are prone to remaining is overcome, the Ru(CH3COO)2(R)-BINAP is an industrial mature catalyst, the technological operation process is not harsh, and large-scale production is easy to achieve.

The invention discloses a preparation process of a hypotensive drug optically pure cilnidipine. The preparation process comprises the following steps: 1) in the presence of (S)-BINAP and a ferric ironcompound, adding ethyl cyano acetoacetate, m-nitrobenzaldehyde and 3-amino-2-methoxyethyl butenoate into isopropanol to react to obtain (R)-1,4-dihydro-2,6-dimethul-4-(3-nitryl phenyl)-3,5-dipicolinic acid-3-(2-cyano ethyl ester)-5-(2-methoxyl ethyl ester); 2) stirring the product in a tetrahydrofuran aqueous solution of alkali to react to obtain (R)-1,4-dihydro-2,6-dimethyl-4-(3-nitryl phenyl)-3,5-dipicolinic acid-5-(2-methoxyl ethyl ester); and 3) carrying out an esterification reaction with cinnamyl alcohol to obtain the optically pure (R)-cilnidipine. The three-step yield of the (R)-cilnidipine reaches up to 41%, ee% reaches up to 99.5%, and the preparation process is simple and suitable for industrial production.

The invention relates to a method for preparing L-carnitine by asymmetric catalytic hydrogenation reduction. Alkyl 4-chloroacetoacetate is used as a raw material, [RuCl(cymene)(S-BINAP)]Cl[chloro[(S)-(-)-2,2'-di(diphenylphosphine)-1,1'-binaphthyl](p-cymene)ruthenium chloride(II))] is used as a catalyst, and amination and hydrolysis reaction are carried out to obtain the L-carnitine product. The amination reaction does not need any solvent or virulent cyanide. The chemical purity of the L-carnitine product is higher than 97%, and the specific rotation [alpha]20D is -29 -32. The invention has the advantages of high reaction speed, stable catalytic system, low pressure required by the reaction process, high conversion rate, no need of solvent in the amination reaction, and is convenient to operate, thereby lowering the cost, reducing the environmental pollution and being convenient for large-scale production.

The invention relates to a phosphine ligand and polyether functionalized ionic liquid integrated chiral catalyst and application thereof in asymmetric catalytic hydrogenation reaction. In an asymmetric hydrogenation reaction, the dual functions of the chiral catalyst and the solvent ionic liquid can be exerted at the same time only by a catalytic amount of phosphine ligand and ionic liquid integrated catalyst; according to the method, the chiral catalyst is recycled and circulated, so that the solvent ionic liquid does not need to be additionally added, the negative effect of the solvent ionicliquid is reduced to the maximum extent, efficient, green and economical utilization of the ionic liquid is realized, and the problem that a large amount of solvent ionic liquid is needed for recycling the chiral catalyst in the prior art is solved.

The invention discloses a preparation method of a multiphase asymmetric catalyst and belongs to the field of synthesis and application of functional materials. The catalyst is prepared from a metal component and a support. A preparation method of the catalyst support comprises the step as follows: a chiral bidentate phosphine ligand BINAP (5, 5'-divinyl-BIANP) containing vinyl is auto-polymerizedor is co-polymerized with other vinyl monomers with high steric hindrance; the metal component in the multiphase catalyst is Rh element. The periphery of the chiral phosphine ligand in a polymer skeleton is modified with other groups, a chiral pocket shown in the description is formed, so that catalytic performance of the multiphase catalyst in asymmetric hydroformylation can be improved, and enantio-selectivity of a product of the catalyst is increased by about 70% as compared with that of a homogeneous catalyst.

A low-cost, feasible and modular method for the preparation of new, highly selective "catalytic membranes" and their use in various types of reactors is disclosed. The membranes are versatile and reusable with negligible catalyst leaching, especially in the asymmetric hydrogenation of substituted α,β-unsaturated acids or esters. The membrane comprises a hybrid inorganic / polymer carrier material (i) and a molecular catalyst (ii) immobilized on the hybrid inorganic / polymer carrier material (i), wherein -(i) consists of an inorganic compound and an organic The hybrid inorganic / macromolecular compound composed of polymer chemical combination; -The inorganic compound is at least one selected from silicic acid compound, tungstic acid compound, molybdic acid compound and stannic acid compound; -The organic polymer Has a hydroxyl group, preferably polyvinyl alcohol (PVA); -(ii) is a pre-formed metal catalyst comprising at least one selected from Ru, Rh, Pd, Ir, Ni, Pt, Au A transition metal and at least one chiral ligand selected from phosphinos, aminos and / or amino-phosphines, preferably DIOP, BINAP monophosphorus or TMBTP.

The invention relates to a synthesis method of a drug for treating leukemia. The synthesis method comprises that 1, a compound 3-methyl-3-oxetanemethanol and sodium metal undergo a reaction to produce 3-sodium methoxide-3-methyl-3-oxetane, 2, 4-amino-3-nitrochlorobenzene is added into the product obtained by the step 1 so that reddish-orange solids (A1) are obtained, a compound 8-benzyloxyquinolin-2-chlorine and A1 undergo a reaction to produce orange solids A2, 3, the compounds A2, 13g of palladium / carbon and formic acid undergo a reaction, formamidine acetate is added into the reaction product, and the mixture is subjected to reflux and drying so that white-like (or yellow) solids A3 are obtained, and 4, the compounds A3 and benzenesulfonyl chloride undergo a reaction, the product is dried to form maize-yellow solids A4, BINAP, A4, tert-butyl piperidin-4-yl-carbamate and potassium carbonate undergo a reaction, the reaction product is dried to form A5, and the A5 is refined through the step 5 so that a pure product is obtained. In the steps 1 and 2, a one-pot method is used.

The invention belongs to the field of medicine synthesis and particularly provides a preparation method for Sitagliptin. According to the method, a cheap metal ruthenium complex and cheap R-BINAP serve as ligands, and the asymmetric hydrogenation reduction of an enamine intermediate is catalyzed, so that R-configuration Sitagliptin can be obtained in a high-selectivity manner; and the reaction time is short, and both the yield of reduction and the ee value of the product are relatively high, so that the method is applicable to industrialized amplified production.