12 results about "Pentamethylcyclopentadiene" patented technology

The invention relates to a preparation method of pentamethylcyclopentadienyl titanium trichloride, which comprises the following steps: S1, vacuumizing a reactor for replacement, detecting the content of moisture and oxygen in gas in the reactor, and stopping vacuum replacement after the content is qualified; s2, adding titanium tetrachloride and methylbenzene into a reactor, dropwise adding a pentamethyl cyclopentadienyl lithium / potassium solution into the reactor, and reacting to obtain a crude product pentamethyl cyclopentadienyl titanium trichloride; s3, the crude product pentamethyl cyclopentadienyl titanium trichloride obtained in the step S2 is filtered, and a crude product pentamethyl cyclopentadienyl titanium trichloride solid is obtained; and S4, adding the crude product pentamethyl cyclopentadienyl titanium trichloride solid obtained in S3 into a mixed solution of toluene and tetrahydrofuran, carrying out hot filtration, and recrystallizing to obtain a pure product pentamethyl cyclopentadienyl titanium trichloride. The pentamethyl cyclopentadienyl titanium trichloride is synthesized in one step, the method is simple, the reaction efficiency is high, and the synthesis process route is shortened.

The invention relates to the technical field of synthesis of aryl acetylene derivatives, in particular to an aryl acetylene derivative as well as a preparation method and application thereof. Comprising the following steps: by taking pentamethylcyclopentadienyl carbonyl cobalt diiodide as a metal catalyst, jointly dissolving N-(substituted phenyl) pivalamide, an alkyne bromide derivative, the metal catalyst, a first silver salt additive and a second silver salt additive in 1, 2-dichloroethane, and performing hydrocarbon activation reaction to obtain an aryl acetylene derivative; wherein the first silver salt additive is silver trifluoromethanesulfonate, silver tetrafluoroborate or silver hexafluoroantimonate; and the second silver salt additive is silver carbonate or silver acetate. According to the preparation method of the aryl acetylene derivative, the aryl acetylene derivative can be efficiently and rapidly synthesized in one step, and the technical problems that traditional reaction conditions are harsh and operation is complex are solved. The method has the advantages of low cost, high yield, simplicity and convenience in operation and no pollution, and has a potential industrial application prospect.

The invention discloses a method for isomerizing trans-1, 2-diarylethene into cis-1, 2-diarylethene, and belongs to the technical field of organic synthesis.The method comprises the steps that in an organic solvent, trans-1, 2-diarylethene serves as a substrate, a rhodium complex serves as a catalyst, an isomerization reaction is conducted in the air atmosphere under visible blue light irradiation, and the cis-1, 2-diarylethene is obtained; the catalyst is 1, 2-diarylethene; the rhodium complex is a pentamethyl cyclopentadienyl rhodium complex coordinated with an eta < 6 >-aromatic ring or a derivative of the pentamethyl cyclopentadienyl rhodium complex; the method is easy to operate, inert gas protection is not needed, additional additives are not needed, the trans-1, 2-diarylethene raw material is rich in source and relatively low in price, and the rhodium complex catalyst can be recycled and accords with the concept of green chemistry. The method provided by the invention provides an efficient and reliable path for the acquisition of cis-1, 2-diarylethene.

The invention discloses a method for synthesizing diphenylamine from aniline. According to the method, aniline is taken as a synthesis raw material, a hydrogen-bridged binuclear iridium complex [Cp * Ir (mu-H) 3IrCp *] [X] (Cp *: pentamethylcyclopentadiene, X: BF4 <->, PF6 <->, BPh4 <-> and CF3SO3 <->) is taken as a catalyst, and the diphenylamine product is obtained under the conditions that the reaction temperature is 100-300 DEG C and the reaction pressure is 0.5-4.0 MPa. According to the method, the aniline conversion rate is high, the diphenylamine selectivity is good, and after the reaction is completed, the catalyst can be recycled in a solvent polarity blending mode.

The invention relates to the technical field of high polymer materials, and particularly provides a syndiotactic polystyrene-methylstyrene copolymer and a preparation method thereof. Comprising the following steps: dissolving pentamethylcyclopentadienyl titanium trichloride in toluene to form a catalyst solution; and mixing tetrahydrofuran, styrene, alpha-methyl styrene, MMAO, n-butyllithium, the catalyst solution and a binuclear scandium catalyst in an inert atmosphere, sequentially carrying out prepolymerization and pressurized main polymerization reaction in a temperature range of room temperature to 80 DEG C, pouring the solution into acidified methanol after the reaction is finished, and carrying out solid-liquid separation and drying to obtain the product. According to the invention, an innovative dual-catalyst system is adopted, pentamethylcyclopentadienyl titanium trichloride and a binuclear scandium catalyst are synergistically utilized, and the copolymer with ideal fluidity is efficiently prepared under optimized reaction conditions.

This invention relates to the field of organometallic complex catalysis, specifically disclosing an organometallic iridium complex capable of efficiently and selectively catalyzing the regeneration of coenzyme NADH and its preparation method. The organometallic iridium complex is a novel pentamethylcyclopentadienyl (Cp*)pyridinesulfonamide iridium complex. The advantage of this invention is that this organometallic iridium complex can efficiently and selectively catalyze the oxidation of coenzyme NAD. + Low-temperature hydrogenation converts it into reduced coenzyme NADH, and it exhibits good biocompatibility.

This invention relates to a method for preparing bis(pentamethylcyclopentadienyl)ruthenium(II), belonging to the field of noble metal organometallic compound synthesis technology. The method involves de-airing a solvent and pentamethylcyclopentadiene to obtain a pretreated solvent and pretreated pentamethylcyclopentadiene, respectively. Under a protective atmosphere, ruthenium chloride is dissolved in the pretreated solvent to obtain a ruthenium solution. A reducing agent and pentamethylcyclopentadiene are added sequentially to the ruthenium solution, and the mixture is heated uniformly to 50-90°C and stirred for 4-10 hours. After cooling and crystallization, the solid and liquid are separated. The solid is washed sequentially with deionized water and methanol, and dried to obtain crude bis(pentamethylcyclopentadienyl)ruthenium(II). The crude bis(pentamethylcyclopentadienyl)ruthenium(II) is dissolved in hot anhydrous ethanol, filtered to remove impurities, and the filtrate is cooled and crystallized. After solid-liquid separation, the solid is dried to obtain high-purity bis(pentamethylcyclopentadienyl)ruthenium(II). This invention has a simple method, a product yield greater than 74%, and a purity of over 98%.

The application discloses a method for synthesizing diphenylamine from aniline. μ -H)3IrCp*][X] (Cp*: pentamethylcyclopentadiene; X: BF4 — , PF6 — , BPh4 — , CF3SO3 — ) as a catalyst, and diphenylamine is obtained under the conditions of a reaction temperature of 100-300 DEG C and a reaction pressure of 0.5-4.0 MPa. The method has high aniline conversion rate and good diphenylamine selectivity, and the catalyst can be recovered through solvent polarity adjustment after the reaction is completed.

This invention belongs to the field of chemical production technology, specifically disclosing a purification method for trimethoxy(pentamethylcyclopentadienyl)titanium, comprising the following steps: vacuum distillation of crude trimethoxy(pentamethylcyclopentadienyl)titanium raw material to obtain a crude distillate; adding 5-20 parts by mass of a modifier to 100 parts by mass of the crude distillate, wherein the modifier is at least one selected from triethylene glycol dibutyl ether, tetraethylene glycol dibutyl ether, n-heptadecane, n-octadecane, and mineral oil, and then distilling to obtain the product. This invention achieves large-scale purification of Star-Ti, achieving a distillation yield of over 75%, with a maximum of over 95%, and obtaining a high-purity product with an organic purity of over 99.5%, solving the problems of difficult large-scale purification, difficulty in purity improvement, and low recovery rate of Star-Ti in existing technologies.

The application discloses rhodium catalytic hydrogen activation for preparation of novel amino acids, and belongs to the technical field of organic synthesis. The method comprises the following steps: adding lysine derivative, disubstituted alkyne, pentamethylcyclopentadienyl rhodium catalyst, cesium acetate and anhydrous copper acetate into a reactor; stirring in a solvent; after the reaction is completed, removing the solvent by using a rotary evaporator to obtain a crude product; and separating the crude product by using a silica gel column chromatography to obtain a target compound. The synthesis method of the novel amino acid has the characteristics of scientific rationality, simple operation, high yield of the target compound, easy purification of the product, fluorescence activity and the like. The reaction equation is as follows.

The application relates to a preparation method of pentamethylcyclopentadienyl tris(methoxy) titanium, which comprises the following steps: S1, carrying out a heating reaction of Ti(NR 1 R 2 )4 and pentamethylcyclopentadiene in the presence of tris(pentafluorophenyl) borane and a solvent; S2, after the reaction in the step S1 is completed, methanol is added to carry out an alcoholysis reaction, after the reaction is completed, the solvent is removed, and the pentamethylcyclopentadienyl tris(methoxy) titanium is obtained. The application takes titanium tetrakis(dimethylamino) compound and pentamethylcyclopentadiene as starting materials, and under the catalysis of a specific and appropriate Lewis acid catalyst tris(pentafluorophenyl) borane, the pentamethylcyclopentadienyl tris(methoxy) titanium can be efficiently reacted to generate pentamethylcyclopentadienyl tris(methoxy) titanium, and the yield is as high as 95%. The method is suitable for industrial large-scale production, and has the advantages of easy raw material, simple operation and good atomic economy; and the whole process does not involve any chlorine-containing reagent, so the deterioration of the chlorine-containing impurities on the electrical properties of the atomic layer deposition film is avoided from the source.

This invention discloses a β ( Z A method for synthesizing alkenylsilanes of type [Cp*Rh( μ -Cl)3RhCp*][X](Cp*:pentamethylcyclopentadienyl; X:Cl ‑ BF4 ‑ CF3SO3 ‑ Complex-catalyzed hydrosilylation of alkynes enables highly regioselective and stereoselective synthesis. β ( Z () type alkenylsilane compounds. The complex catalyst used in this invention can be recovered and reused by adding a weakly polar solvent to the reaction product and then filtering; at the same time, this invention overcomes the... β ( Z The synthesis of alkenylsilanes is difficult due to their thermodynamic instability. However, the reaction conditions are mild and the operation is simple, making them promising for future applications.