51 results about "Dibenzylideneacetone" patented technology

The invention discloses an anthracene nitrogen-containing organic light-emitting compound and a preparation method and application thereof, the specific structure of the anthracene nitrogen-containingorganic light-emitting compound is as shown in the general formula 1 in the specification, and the preparation method comprises the following steps: taking methylbenzene as a solvent; reacting the raw material A with the raw material B in the presence of sodium tert-butoxide, tris (dibenzylideneacetone) dipalladium and tris(tert-butyl)phosphorus to obtain an intermediate product C, reacting the intermediate product C with NBS by taking dichloromethane as a solvent to obtain an intermediate product D, and reacting the intermediate product D with a mixed solution of methylbenzene, ethanol and water by taking a mixed solution of methylbenzene, ethanol and water as a solvent; and reacting the intermediate product D with a raw material E in the presence of potassium carbonate and tetrakis(triphenylphosphine)palladium to finally obtain the compound shown in the general formula I. The anthracene derivative provided by the invention has relatively high electron transmission performance, and can improve the electron transmission efficiency of a device and can prolong the service life of the device when being applied to an organic electroluminescent device. In addition, the preparation method provided by the invention is simple, easy to operate and suitable for industrial popularization.

The invention discloses polyamide thermofuse with a low melting point and a preparation method thereof. A polymerization reaction is conducted by using polyatomic acid and polyamine as reagents, and meanwhile auxiliaries such as modifier, palladium catalyst and defoamer are added; the polyatomic acid is the mixture of oxalic acid, sebacic acid and dodecanedioic acid; the polyamine is the mixture of decamethylene diamine, PA-12 and N-(3-aminopropyl)-N-dodecyl-1; the modifier is the mixture of N-benzyl-4-trifluoromethyl phenylmethylamine and 4,4'-diaminodiphenyl ether; the palladium catalyst isbis(dibenzylideneacetone)palladium or tris(dibenzylideneacetone)dipalladium; and the defoamer is polydimethylsiloxane or ethylene glycol siloxane. The prepared thermofuse has the low melting point, and meanwhile has large intensity and elongation, still has the large intensity and elongation even being irradiated with ultraviolet light for a long time, and can meet actual needs of production and life.

The invention relates to the field of organic chemistry, and discloses a quinazoline derivative, a preparation method and application thereof. The derivative has a structure represented by formula (1). The method provided by the invention comprises: under alkaline condition, in ligand and selected from palladium trifluoroacetate, tetrakis (triphenylphosphine) palladium, bistriphenylphosphine palladium dichloride, three (dibenzylidene acetone) ) In the presence of at least one catalyst in dipalladium and palladium acetate, the compound shown in formula (I) is reacted with the compound shown in formula (II), and the ligand is 2-bicyclohexylphosphine-2', 6'-Dimethoxybiphenyl. The quinazoline derivatives provided by the invention have excellent antibacterial activity and antitumor activity. The preparation method provided by the invention has high yield, wide substrate applicability, mild reaction conditions, simple operation, low cost, few by-products, high product purity, is applicable to large-scale preparation, and has considerable application prospects.

The invention discloses a diphenyl[c,e]azepine derivative and a preparation method thereof, by reacting [1,1'-biphenyl]-2,2'-dinitrile and arylboronic acid The reactant is prepared by the reaction of the reactant; the reactant is easy to prepare, has wide sources, low cost, low toxicity, and is not easy to affect human health. The reaction is carried out in a solvent, and the solvent is any one of toluene, xylene, methanol, tetrahydrofuran, N,N-dimethylformamide and N,N-dimethylacetamide; Added palladium catalyst and acid accelerator; palladium catalyst is palladium trifluoroacetate, palladium tetraphenylphosphine, bisacetylacetonate palladium, bis(dibenzylideneacetone) palladium and tris(dibenzylideneacetone) dipalladium Any one; the reaction temperature is 100-120°C, the reaction time is 20-30 hours, the reaction conditions are mild, easy to achieve, and safe. The invention can directly synthesize the target product without separating intermediate products, and the highest yield can reach 95%.

The invention discloses a preparation method of 4,5-difluorophthalic acid, the specific method steps are as follows: S1: Synthesis of 4,5-difluoro-1,2-phthalonitrile: add 4,5 ‑Difluoro‑1,2‑dihalobenzene and polymethylhydrogensiloxane, stirred and dissolved with N,N‑dimethylacetamide, and reacted, cooled after the reaction, and added tri( Dibenzylideneacetone) dipalladium and 1,1'-bis(diphenylphosphino)ferrocene, then slowly add zinc cyanide for reaction, after the reaction is completed, cool down and add water, and use sodium bicarbonate solution under vigorous stirring Adjust the pH to 8, stir for 2 hours and then filter, wash and elute with a mixed solvent of petroleum ether and ethyl acetate to obtain an off-white solid intermediate 4,5-difluoro-1,2-phthalonitrile; S2: Synthesis of 4,5‑difluoro‑1,2‑phthalic acid. The process of the invention is safe, efficient and easy to operate, has low requirements on equipment, low cost of raw materials, and is easy for industrialized production.

The present invention relates to the design and synthesis of a class of novel chiral phosphine ligand, 1,2-bis(diphenylphosphinoalkylamido)-1,2-disubstituted ethane, and use in asymmetric catalytic reactions, such as asymmetric catalytic synthesis of pyrazoline-5-one with a chiral quaternary carbon center, i.e., highly enantioselective synthesis of 3-methyl-4-benzyl-4-(2-butyl-2,3-butadienyl)pyrazoline-5-one by using 3-methyl-4-benzylpyrazoline-5-one and benzyl (2-butyl-2,3-butadienyl) carbonate with tris(dibenzylideneacetone)dipalladium-chloroform adduct and this novel ligand as catalysts. The ligand designed by this present invention has the following advantages: the structure is novel, the synthesis and enlarge are simple, the enantioselective control effect in the practical reaction is excellent, which has a broad application prospect in chiral catalysis.

The invention provides a synthesis method of a trifluorostyrene compound. According to the method provided by the invention, the trifluorostyrene compound can be synthesized from an accessible fluorin containing raw material and various substituted arylboronic acid compounds in an alkali condition by using a phosphine ligand or a multiphosphine ligand and using bis(dibenzylideneacetone)dipalladium as a catalyst. By adopting the method provided by the invention, the fluorine spectrum yield is extremely improved, while the use amount of the catalyst is obviously reduced.

The invention discloses the structure, synthesis and application of a spirobifluorene hole transport material. The hole transport material is a spirobifluorene hole transport material. The preparation steps are as follows: compound 1, spirobifluorene, t- The mixed system of sodium butoxide, tri-tert-butylphosphine, tris(dibenzylideneacetone) dipalladium and anhydrous toluene is heated to 105-115°C under the protection of argon, and the temperature is maintained for 10-14 hours; after cooling The organic phase was extracted with ethyl acetate, and the organic phase was dried and concentrated, followed by silica gel column chromatography to obtain the target product 2,4‑spiro‑OMeTAD. The hole transport material 2,4-spiro-OMeTAD of the present invention has high hole mobility, the HOMO energy level matches the valence band of perovskite, good stability, good solubility, and high molar extinction coefficient, and the perovskite made of it The photoelectric conversion efficiency of the mineral solar cell is high; the flexible change of its methyl position facilitates structural modification in the later stage, and it is easy to realize spectral absorption in the ultraviolet to near-infrared light region; and the commercialization cost is low.

The invention discloses a preparation method of tris(dibenzylideneacetone)dipalladium(0). The method comprises: 1. Under a nitrogen atmosphere, the ligand dibenzylideneacetone, palladium dichloride and anhydrous Sodium acetate is added in the dehydrated alcohol of stirring state and heated reaction, obtains solid bis (dibenzylidene acetone) palladium (0) after filtration; Two, under nitrogen atmosphere, the solid bis (dibenzylidene acetone) that obtains in step Acetone)palladium(0) was added into acetone in a stirring state for reaction, the retentate was washed after filtration, and the washed retentate was dried to obtain tris(dibenzylideneacetone)dipalladium(0). The present invention adopts dehydrated alcohol, dibenzylidene acetone, palladium dichloride and anhydrous sodium acetate to first prepare bis(dibenzylidene acetone) palladium (0), and then obtains tris(dibenzylidene acetone) through acetone solution treatment ) dipalladium (0), the three (dibenzylideneacetone) dipalladium (0) obtained has higher purity.

A method for preparing a radiotracer precursor SnADAM is revealed. The method overcomes shortcomings of conventional synthesis methods including lower yield rate and time-consuming. Moreover, Pd / C catalyst and hydrogen gas are used to catalyze reduction reaction for avoiding the generation of a large amount of intermediate products with similar structures. Thus there is no need to perform isolation and purification processes. The yield rate of the intermediate products is also increased so that its impact on the low yield rate of the final product SnADAM is minimized. A part of the reaction is significantly accelerated by using tris(dibenzylideneacetone)-dipalladium(0) (Pd2(dba)3) as a catalyst. Thus the production time of SnADAM is shortened.

The present invention provides a process for the preparation of Pd2(dba)3.CHCl3 comprising the steps of: (a) reacting a Pd(II) complex with an alkali metal halide in at least one alcohol solvent; and (b) reacting the product of step (a) with a mixture comprising dibenzylideneacetone, chloroform and an inorganic base to form Pd2(dba)3.CHCl3.