1031246-43-1Relevant academic research and scientific papers
Heterogeneously Catalyzed Selective Decarbonylation of Aldehydes by CeO2-Supported Highly Dispersed Non-Electron-Rich Ni(0) Nanospecies
Matsuyama, Takehiro,Yatabe, Takafumi,Yabe, Tomohiro,Yamaguchi, Kazuya
, p. 13745 - 13751 (2021/11/17)
Aldehyde decarbonylation has been extensively investigated, primarily using noble-metal catalysts; however, nonprecious-base-metal-catalyzed aldehyde decarbonylation has been hardly reported. We have established an efficient selective aldehyde decarbonylation reaction with a broad substrate scope and functional group tolerance utilizing a heterogeneous Ni(0) nanospecies catalyst supported on CeO2. The high catalytic performance is attributable to the highly dispersed and non-electron-rich Ni(0) nanospecies, which possibly suppress a side reaction producing esters and adsorbed CO-derived inhibition of the catalytic turnover, according to detailed catalyst characterization and kinetic evaluation.
Synthetic method of rosuvastatin calcium key intermediate
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Paragraph 0040; 0041; 0042, (2016/10/10)
The invention discloses a synthetic method of a rosuvastatin calcium key intermediate. The synthetic method particularly comprises the following steps: carrying out a condensation reaction between fluoroacetophenone and ethyl isobutyrate under the condition of using sodium as alkali by using isopropyl alcohol as a solvent to prepare 1-(4-fluorophenyl)-4-methyl amyl-1,3-diketone; then carrying out a ring closing reaction between the 1-(4-fluorophenyl)-4-methyl amyl-1,3-diketone and methylguanidine hydrochloride by using isopropanol as a solvent to obtain 4-(4-fluorophenyl)-6-isopropyl-N-methyl pyrimidine-2-amine; carrying out a substitution reaction between the 4-(4-fluorophenyl)-6-isopropyl-N-methyl pyrimidine-2-amine and methanesulfonyl chloride by using dichloromethane as a solvent to obtain 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methanesulfonyl) amino] pyrimidine; finally, carrying out a Vilsmeier reaction between the 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methanesulfonyl) amidogen] pyrimidine and DMF (Dimethyl Formamide) as well as phosphoryl chloride to obtain a target compound. The method disclosed by the invention has the advantages of being simple to operate, low in raw material price, high in availability of used raw materials, mild in reaction conditions, low in equipment requirements and production cost, easy for scale production and the like, and has significance industrial application value.
Method used for synthesizing rosuvastatin calcium key intermediate
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Paragraph 0016; 0035; 0036; 0037, (2016/10/10)
The invention discloses a method used for synthesizing a rosuvastatin calcium intermediate represented by formula I. The reaction route is disclosed in the invention. Raw materials used in the method are low in toxicity; synchronous recycling of used solvents can be realized; expensive materials such as 4-methylmorpholine-N-oxide, TPAP (tetrapropylammonium perruthenate), and DIBAL-H are not used, so that production cost is reduced effectively; reaction conditions are mild; energy consumption is low; no special reaction equipment is needed; operation is simple; one-pot preparation can be realized; and the method is convenient for large-scale production.
Preparation method of rosuvastatin calcium key intermediate
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Paragraph 0033; 0034; 0035, (2016/12/22)
The invention discloses a preparation method of a rosuvastatin calcium key intermediate, i.e. a compound as shown in a formula I. The preparation method comprises the following steps: a, carrying out a reaction between fluoroacetophenone and ethyl isobutyrate to prepare a compound as shown in a formula IV; b, carrying out a reaction between the obtained compound IV and methylguanidine hydrochloride as well as potassium hydroxide to obtain a compound as shown in a formula III; c, carrying out a reaction between the compound III and triethylamine as well as methanesulfonyl chloride to prepare a compound as shown in a formula II; d, carrying out a reaction between the compound as shown in the formula II and N,N-dimethylformamide as well as phosphorus oxychloride to obtain the compound as shown in the formula I. A reaction route of the preparation method is as shown in the following: (referring to the specification). The method disclosed by the invention has the advantages of being simple to operate, low in raw material price, high in availability of used raw materials, mild in reaction conditions, low in equipment requirements and production cost, easy for scale production and the like, and has significance industrial application value.
PROCESS FOR PREPARING PYRIMIDINE DERIVATIVES
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Page/Page column 14-15, (2009/04/25)
The present invention relates to a process for preparing pyrimidine derivatives, in particular as intermediates useful for preparing pyrimidine derivatives of a class that is effective at inhibiting the biosynthesis of cholesterol in humans, such as HMG-CoA reductase inhibitors, e.g. rosuvastatin.
A new approach to the total synthesis of rosuvastatin
Andrushko, Natalia,Andrushko, Vasyl,Koenig, Gerd,Spannenberg, Anke,Boerner, Armin
experimental part, p. 847 - 853 (2009/04/11)
A new multi-step synthesis of the lipid-lowering agent rosuvastatin, involving two homogeneously catalyzed reaction steps, is described. The key building block, N-[4-(4-fluorophenyl)-5-formyl-6-isopropylpyrimidin-2-yl]-N- methylmethanesulfonamide (2), was prepared by Pd-catalyzed formylation with CO/H2 (1:1, 50 bar, phosphane ligand/substrate ratio of 1:10). Several alternative pathways for the preparation of 2 were also tested, but were found to be inferior. Rosuvastatin precursor 1 was assembled by Wittig coupling of aldehyde 2 and ylide (R)-3, derived from a Rucatalyzed asymmetric hydrogenation. The second stereogenic center was finally created by stereoselective reduction with Et2BOMe and NaBH4 to afford rosuvastatin ethyl ester. Wiley-VCH Verlag GmbH & Co. KGaA, 2008.
