3 results about "Tert-Butyllithium" patented technology

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.

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.