865-50-9Relevant articles and documents
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Nolin
, p. 1 (1954)
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Selective Catalytic Frustrated Lewis Pair Hydrogenation of CO2 in the Presence of Silylhalides
Grimme, Stefan,Jupp, Andrew R.,Qu, Zheng-Wang,Stephan, Douglas W.,Wang, Tongtong,Xu, Maotong
supporting information, p. 25771 - 25775 (2021/11/09)
The frustrated Lewis pair (FLP) derived from 2,6-lutidine and B(C6F5)3 is shown to mediate the catalytic hydrogenation of CO2 using H2 as the reductant and a silylhalide as an oxophile. The nature of the products can be controlled with the judicious selection of the silylhalide and the solvent. In this fashion, this metal-free catalysis affords avenues to the selective formation of the disilylacetal (R3SiOCH2OSiR3), methoxysilane (R3SiOCH3), methyliodide (CH3I) and methane (CH4) under mild conditions. DFT studies illuminate the complexities of the mechanism and account for the observed selectivity.
Method for efficiently preparing deuterated iodomethane and application of deuterated iodomethane
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Paragraph 0020; 0022; 0024; 0026; 0028; 0030; 0032, (2021/08/07)
The invention discloses a method for efficiently preparing deuterated iodomethane and an application of the deuterated iodomethane; according to the method, deuterated methanol and iodine elementary substance are used as reaction raw materials, in a hydrogen atmosphere, a transition metal catalyst and a ligand are added, and the deuterated iodomethane is generated in situ at the temperature of 0 DEG C-120 DEG C. The application is the application of deuterated iodomethane as a methylation reagent in preparation of S-(methyl-D3)homocysteine, and mainly comprises the steps: carrying out methylation reaction on a compound a, namely (t-butyloxycarboryl)-L-homocysteine methyl ester and deuterated iodomethane in an organic solvent under the action of a base catalyst to obtain a product b; and performing deprotection on the product b to obtain a target product c, namely S-(methyl-D3)homocysteine. Anhydrous hydrogen iodide is prepared through catalysis of a transition metal catalyst, the anhydrous hydrogen iodide and deuterated methanol directly react through a one-pot method to obtain deuterated iodomethane with the high yield (88%), and the deuterated iodomethane serves as a deuterated methyl reagent to prepare S-(methyl-D3)homocysteine with the high deuterium doping rate and the yield (75%). The method is simple and easy to operate, and reaction conditions are mild.
A stable isotope labeled β receptor agonist synthetic method of compound
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Paragraph 0064-0065; 0075; 0076; 0085; 0086; 0090; 0091, (2017/04/29)
The invention relates to a synthesis method of a stable isotope-labeled beta receptor agonist type compound. The synthesis method comprises the following steps: (1) by taking stable isotope-labeled methanol as a raw material, reacting with acetone or stable isotope-labeled acetone, and ammonifying to obtain stable isotope-labeled tert-butylamine; and (2) by taking a bromoketone type compound as a precursor of the beta receptor agonist type compound, reacting with stable isotope-labeled tert-butylamine to prepare the stable isotope-labeled beta receptor agonist type compound. Compared with the prior art, the method for preparing the stable isotope-labeled beta receptor agonist, provided by the invention, is simple, safe and reliable, the chemical purity of the product after separation and purification is above 99.0%, the isotopic abundance is above 98.0% atom, and the product can fully meet the requirements of residual detection in the field of food safety.