- Selective Catalytic Frustrated Lewis Pair Hydrogenation of CO2 in the Presence of Silylhalides
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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.
- Grimme, Stefan,Jupp, Andrew R.,Qu, Zheng-Wang,Stephan, Douglas W.,Wang, Tongtong,Xu, Maotong
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supporting information
p. 25771 - 25775
(2021/11/09)
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- A stable isotope labeled β receptor agonist synthetic method of compound
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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.
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Paragraph 0069; 0070; 0071
(2017/04/29)
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- The first synthesis of [11C]SB-216763, a new potential PET agent for imaging of glycogen synthase kinase-3 (GSK-3)
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SB-216763 is a novel, potent and selective glycogen synthase kinase-3 (GSK-3) inhibitor with an IC50 value of 34 nM. [11C]SB- 216763 (3-(2,4-dichlorophenyl)-4-(1-[11C]methyl-1H-indol-3-yl)-1H- pyrrole-2,5-dione), a new potential PET agent for imaging of GSK-3, was first designed and synthesized in 20-30% decay corrected radiochemical yield and 370-555 GBq/μmol specific activity at end of bombardment (EOB). The synthetic strategy was to prepare a carbon-11-labeled maleic anhydride intermediate followed by the conversion to maleimide.
- Wang, Min,Gao, Mingzhang,Miller, Kathy D.,Sledge, George W.,Hutchins, Gary D.,Zheng, Qi-Huang
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experimental part
p. 245 - 249
(2011/02/27)
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- Synthesis of [1-11C]ethyl iodide from [11C]carbon monoxide and its application in alkylation reactions
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A method is presented for preparing [1-11C]ethyl iodide from [11C]carbon monoxide. The method utilizes methyl iodide and [ 11C]carbon monoxide in a palladium-mediated carbonylation reaction to form a mixture of [1-11C]acetic acid and [1-11C]methyl acetate. The acetates are reduced to [1-11C]ethanol and subsequently converted to [1-11C]ethyl iodide. The synthesis time was 20 min and the decay-corrected radio-chemical yield of [1-11C]ethyl iodide was 55 ± 5%. The position of the label was confirmed by 13C- labelling and 13C-NMR analysis. [1-11C]Ethyl iodide was used in two model reactions, an O-alkylation and an N-alkylation. Starting with approximately 2.5 GBq of [11C]carbon monoxide, the isolated decay-corrected radiochemical yields for the ester and the amine derivatives were 45 ± 0.5% and 25 ± 2%, respectively, based on [ 11C]carbon monoxide. Starting with 10 GBq of [11C]carbon monoxide, 0.55 GBq of the labelled ester was isolated within 40 min with a specific radioactivity of 36 GBq/μmol. Copyright
- Eriksson, Jonas,Antoni, Gunnar,Langstroem, Bengt
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p. 723 - 731
(2007/10/03)
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- Large-scale preparation of [13C]methyl phenyl sulfide from [13C]methanol by a one-step process
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We have developed a large-scale "one-pot" procedure for the conversion of commercially available [13C]- or [2H3,13C]-methanol to [13C]- or [2H3,13C]methyl phenyl sulfide. [13C]methyl phenyl sulfide is a potentially versatile, chemically stable, and nonvolatile labeling precursor. In addition, we report an efficient method for the oxidation of [13C]methyl phenyl sulfide to [13C]methyl phenyl sulfone. Finally, we have used [13C]methyl phenyl sulfide to produce 13C-labeled methyl iodide, containing exactly one or two deuterons.
- Martinez, Rodolfo A.,Alvarez, Marc A.,Velarde, Stephen P.,Silks, Louis A. Pete,Stotter, Philip L.,Schmidt, Juergen G.,Unkefer, Clifford J.
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p. 851 - 854
(2013/09/06)
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