- Preparation method for bis[di-tert-butyl(4-dimethylaminophenyl)phosphine]dichloropalladium
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The invention discloses a preparation method for bis[di-tert-butyl(4-dimethylaminophenyl)phosphine]dichloropalladium. The preparation method comprises the following steps that 1, a Grignard reagent isprepared from the raw materials of N, N-dimethyl p-haloaniline and magnesium chips; 2, the Grignard reagent is taken and cooled, then a catalyst is added for reaction, then di-tert-butylchlorophosphane is dropwise added, and heating is carried out for reaction so as to obtain di-tert-butyl-4-dimethylaminophenylphosphine; 3, the di-tert-butyl-4-dimethylaminophenylphosphine is purified; and 4, complexing bis(acetonitrile)dichloropalladium and the purified di-tert-butyl-4-dimethylaminophenylphosphine so as to obtain a target product. The preparation method has the advantages that the di-tert-butyl-4-dimethylaminophenylphosphine is purified, the high-purity di-tert-butyl-4-dimethylaminophenylphosphine is used for reacting with the bis(acetonitrile)dichloropalladium, and therefore the yield loss of the noble metal palladium is greatly reduced, the preparation cost is greatly lowered, and the method has a good practical value.
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Paragraph 0062; 0063
(2018/11/03)
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- Nickel-Catalyzed Cross-Coupling of Functionalized Organo manganese Reagents with Aryl and Heteroaryl Halides Promoted by 4-Fluorostyrene
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A catalytic system consisting of Ni(acac) 2 (5 mol%) and 4-fluorostyrene (20 mol%) allows a convenient cross-coupling of functionalized organomanganese reagents with a variety of aryl and heteroaryl halides leading to polyfunctionalized diaryl- and arylheteroarylmethane derivatives.
- Benischke, Andreas D.,Desaintjean, Alexandre,Juli, Thomas,Cahiez, Gérard,Knochel, Paul
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supporting information
p. 5396 - 5412
(2017/12/14)
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- Selective introducing of aryl and amino groups: Reaction of benzanthrone and organometallic reagents
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The reaction of benzanthrone and aryl magnesium bromides produced 6-aryl-substituted benzanthrones in moderate to good yields. Similarly, 6-alkylaminobenzanthrones were selectively prepared by the reaction of benzanthrone and lithium alkylamides. In contrast, for the lithium arylamides, the arylamino groups were selectively introduced at the 4-position of the benzanthrone.
- Umeda, Rui,Namba, Teruaki,Yoshimura, Tomohiro,Nakatsukasa, Masamichi,Nishiyama, Yutaka
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p. 1526 - 1531
(2013/02/23)
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- Cross-coupling of aryl/alkenyl silyl ethers with grignard reagents through nickel-catalyzed CO bond activation
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CO activation and its application have drawn much attention since oxygen-based electrophiles are easily available, less toxic, and more environmentally benign. This letter presents systematically results on the Ni-catalyzed KumadaTamaoCorriu coupling based on siloxy arenes/alkenes, which provides a new strategy of silyl protection/CC bond formation sequence in organic synthesis.
- Zhao, Fei,Yu, Da-Gang,Zhu, Ru-Yi,Xi, Zhenfeng,Shi, Zhang-Jie
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supporting information; experimental part
p. 1001 - 1003
(2011/12/05)
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- CATALYTIC RADIOFLUORINATION
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One aspect of the present invention relates to a method of preparing radio fluorinated substituted alkyl, cycloalkyl, aryl, and alkenyl compounds. In a preferred embodiment, potassium fluoride-18 is used. Another aspect of the invention relates to arylammonium compounds containing fluorine-18 that are useful as imaging agents. In certain embodiments, the ammonium compound is a tetraaryl ammonium salt. Another aspect of the invention relates to arylsulfonium compounds containing fluorine-18 that are useful as imaging agents. In certain embodiments, the sulfonium compound is a triaryl sulfonium salt. Another aspect of the present invention relates to a method of obtaining a positron emission image of a mammal, comprising the steps of administering to a mammal a compound of the invention, and acquiring a positron emission spectrum of the mammal.
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Page/Page column 94-95
(2010/11/30)
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- Arylzinc species by microwave assisted Grignard formation-transmetallation sequence: Application in the Negishi coupling
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Arylmagnesium species can be efficiently generated from magnesium turnings and aryl chlorides or aryl bromides under dielectric heating conditions. Subsequent microwave assisted transmetallation using ZnCl2-TMEDA afforded the corresponding arylzinc reagents. A sequential microwave assisted arylmagnesium formation-transmetallation-Negishi coupling protocol suitable for automated multiple parallel synthesis has been developed.
- Mutule, Ilga,Suna, Edgars
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p. 11168 - 11176
(2007/10/03)
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- Activation of Mg metal for safe formation of Grignard reagents on plant scale
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A general and reliable method for the activation of magnesium metal for the formation of various kinds of Grignard reagents has been developed. Utilizing diisobutylaluminum hydride (DIBAH) for the activation of the surface and drying of the reaction mixtu
- Tilstam, Ulf,Weinmann, Hilmar
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p. 906 - 910
(2013/09/06)
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- Effect of a 17α-(3-hydroxypropyl)-17β-acetyl substituent pattern on the glucocorticoid and progestin receptor binding of 11β-arylestra-4,9-dien-3-ones
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(matrix presented) Replacing the 17α-acetoxy substituent in an antiprogestational 17β-acetyl-11β-arylestra-4,9-dien-3-one by 3-hydroxypropyl significantly diminished glucocorticoid receptor binding with little effect on progestin receptor binding.
- Cook, C. Edgar,Raje, Prasad,Lee, David Y.-W.,Kepler, John A.
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p. 1013 - 1016
(2007/10/03)
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