6 results about "Tert-Butyllithium" patented technology

The invention discloses a novel method for synthesizing a ferrocenyl phosphine ligand compound, which comprises the following steps of: reacting a ferrocene compound serving as a starting material with a Grignard reagent and phosphorus trichloride under the action of tert-butyl lithium to generate a ferrocene phosphine ligand, and synthesizing a ferrocene diphosphine ligand in one step. The method is stable and high in practicability, and a novel method for synthesizing the ferrocene ligand compound is provided.

The invention relates to the technical field of tert-butyllithium preparation, in particular to a tert-butyllithium preparation method which comprises the following steps: preparing raw materials, dissolving lithium and washing oil, mixing the raw materials to start reaction, dropwise adding a modifier, carrying out heat preservation treatment, cooling, settling and taking clear liquid. According to the method, trace impurities on the surface of lithium are removed in the pretreatment link, the PVP coating can block contact of water, oxygen and lithium in a long-acting mode, lithium is prevented from going bad in the earlier stage of storage and reaction, and meanwhile the compatibility of lithium and organic solvents such as n-pentane is enhanced; the interference of impurities on the reaction can be eliminated in a high-purity state of the chlorinated tert-butane, byproducts such as lithium tert-butoxide are prevented from being generated, the moisture in the system is strictly limited by deep dehydration, a stable anhydrous environment is provided for synthesis of the tert-butyllithium, and the reaction efficiency is guaranteed; the operation of deep dehydration and impurity removal by activated aluminum oxide creates a high-cleanliness solvent system for the reaction, avoids the action of water and polar impurities with tert-butyllithium or reaction intermediates, and prevents product decomposition or impurity generation.

The invention discloses a synthesis method of 3-amino-2-(tert-butyldimethylsilyl) phenyl trifluoromethanesulfonate, which is characterized in that a compound 2-bromo-3-nitrophenol is used as a raw material, and the target compound 3-amino-2-(tert-butyldimethylsilyl) phenyl trifluoromethanesulfonate is obtained through four-step reaction. According to the synthesis method disclosed by the invention, tert-butyllithium which is commonly used in the prior art is not used in key steps, and bis (trimethylsilyl) amino lithium (LiHMDS) is adopted to convert a compound 3, namely, 2-bromo-3-((tert-butyldimethylsilyl) oxy) aniline into a compound 4, namely, 3-amino-2-(tert-butyldimethylsilyl) phenol; the reaction risk is greatly reduced, meanwhile, the reaction effect is remarkably improved, no by-product is generated, post-treatment and purification are simple, and the yield is ideal.

The invention relates to the technical field of catalysis, in particular to a catalyst system for synthesizing butyraldehyde through hydroformylation and application of the catalyst system. The invention relates to a catalyst system for synthesizing butyraldehyde through hydroformylation. The catalyst system comprises a first ligand, a second ligand and a metal active component, the first ligand is a bidentate rigid phosphine ligand, and the second ligand is a monodentate auxiliary phosphine ligand; the preparation method of the first ligand comprises the following steps: 1) reacting o-bromotoluene, tert-butyl lithium and diphenyl phosphine chloride to obtain o-tert-butyl diphenyl phosphine; (2) carrying out electrophilic substitution reaction on o-tert-butyl diphenylphosphine and silver trifluoromethanesulfonate to introduce-CF3 groups to benzene ring para-positions; then, purification is carried out, and o-tert-butyl-p-trifluoromethyl diphenylphosphine is obtained; 3, tert-butyl-p-trifluoromethyl diphenylphosphine reacts with 1, 2-dibromoethane to generate a bidentate ligand, then recrystallization purification is conducted, and the first ligand is obtained.When the first ligand is applied to a reaction for synthesizing butyraldehyde through hydroformylation, the normal / isomeric ratio of the obtained product can reach 25.4-30: 1.

This invention discloses a norbornene skeleton monophosphine ligand, its borane adduct, palladium complex, its preparation method, and its application. The norbornene skeleton monophosphine ligand is prepared through the following steps: using a palladium metal complex as a catalyst, and triethylamine and formic acid as negative hydrogen sources, in a solvent, bromonorbornene and its analogues undergo a hydroarylation reaction with ArX, where X in ArX is I, Br, or OTf, to obtain an aryl-substituted bromonorbornene skeleton. The aryl-substituted bromonorbornene skeleton undergoes a lithium bromide exchange with tert-butyllithium, followed by R... 1 R 2 PCl undergoes a substitution reaction to prepare the norcamphor skeleton monophosphine ligand, and the norcamphor skeleton monophosphine ligand-palladium complex exhibits good catalytic activity in the Suzuki coupling reaction.

This application relates to the field of catalytic technology, in particular to a catalyst system for hydroformylation synthesis of butyraldehyde and its application. A catalyst system for hydroformylation synthesis of butyraldehyde includes a first ligand, a second ligand and a metal active component; the first ligand is a bidentate rigid phosphine ligand, and the second ligand is a monodentate auxiliary phosphine ligand; the preparation method of the first ligand is as follows: 1) React o-bromotoluene, tert-butyllithium and diphenylphosphine chloride to obtain o-tert-butyldiphenylphosphine; 2) Carry out an electrophilic substitution reaction between o-tert-butyldiphenylphosphine and silver trifluoromethanesulfonate to introduce a -CF3 group at the para position of the benzene ring; then purify to obtain o-tert-butyl-p-trifluoromethyl diphenylphosphine; 3) React tert-butyl-p-trifluoromethyl diphenylphosphine with 1,2-dibromoethane to generate a bidentate ligand, and then purify by recrystallization to obtain the first ligand. When it is applied to the hydroformylation synthesis of butyraldehyde reaction, the n / i ratio of the obtained product can reach 25.4 - 30:1.