- 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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- Method for synthesizing [4-(N,N-dimethylamino)phenyl]dialkylphosphine
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The invention discloses a method for synthesizing [4-(N,N-dimethylamino)phenyl]dialkylphosphine and belongs to the field of organic synthesis. According to the method, N,N-dimethylaniline as a raw material and 4-dimethylamino-pyridine as a base are reacted, in water-free oxygen-free atmosphere, with dialkyl phosphorous chloride under the catalytic action of cuprous acetate to generate [4-(N,N-dimethylamino)phenyl]dialkylphosphine. Compared with the prior art, the method has the advantages that reaction conditions are mild, operating is simple, the yield is high, the materials are simple and easy to obtain, production cost is reduced and the method is suitable for industrial production.
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Paragraph 0009; 0010
(2017/10/31)
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- Di-tert-butyl - 4 - dimethyl amino phosphonate and double (di-tert-butyl - 4 - dimethyl amino phosphonate) preparation method of catalysts
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The invention provides a preparing method for di-tertiary butyl-4-dimethylamino phenylphosphine. Di-tertiary butylphosphine is subjected to low-temperature lithiation under shielding of inert gas and then reacts with N,N-dimethyl p-chloroaniline, and di-tertiary butyl-4-dimethylamino phenylphosphine is obtained. According to the preparing method, di-tertiary butyl-4-dimethylamino phenylphosphine is purified after a quenching reaction. The invention further provides a preparing method for bis(di-tertiary butyl-4-dimethylamino phenylphosphine) palladium chloride. Di-tertiary butyl-4-dimethylamino phenylphosphine obtained through the preparing method is further subjected to complexation with (1,5-cyclooctadiene) palladium dichloride or bispalladium dichloride. A di-tertiary butyl-4-dimethylamino phenylphosphine ligand is prepared through the novel method, purified and then subjected to palladium complexation, and the preparing yield is greatly increased; meanwhile, the loss of palladium is reduced, the preparing cost is greatly reduced, and the obtained products are high in purity and good in quality.
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Paragraph 0061-0063
(2017/08/25)
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- NOVEL CATALYSTS
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The present invention provides novel compounds and ligands that are useful in transition metal catalyzed cross-coupling reactions. For example, the compounds and ligands of the present invention are useful in palladium or gold catalyzed cross-coupling reactions.
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Page/Page column 71
(2012/06/01)
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