2-氯甲基-4-甲氧基-3,5-二甲基吡啶的合成方法改进

采用POCl3/CH2Cl2/Et3N体系作为选择性氯化试剂,以2,3,5-三甲基吡啶为起始原料,方便、高产率地合成了2-氯甲基-4-甲氧基-3,5-二甲基吡啶。其结构经1HNMR和IR确证。     

Synthesis and biological activity of 3,5-diacetyl-2,6-dimethylpyridine derivatives

Chemistry of Heterocyclic Compounds - Aldol-crotonic condensation reactions of 3,5-diacetyl-2,6-dimethylpyridine with various aldehydes were used to synthesize bisazachalcone derivatives, which...     

Synthesis of 2-phenylindole N-derivatives under conditions of catalysis by palladium complexes

The synthesis of 2-phenylindole N-derivatives was accomplished. The synthesis included the catalytic coupling of o-iodoaniline with phenylacetylene leading to 2-aminotolan, the preparation of the derivative of the last at the nitrogen atom, and its catalytic cyclization to the corresponding indole.M. V. Lomonosov Moscow State University, Moscow 119899, Russia. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 2, pp. 194–198, February, 1999.     

Mild alkoxycarbonylation of olefins in the presence of palladium complexes

Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 3, p. 743, March, 1989.     

Conversion of 4-hydroxy-3,5-di-tert-butylbenzonitrile to palladium and rhodium complexes

Conclusions Complexes of palladium (II) and rhodium (III) with 4-hydroxy-3,5-di-tert-butylbenzo-nitrile have been synthesized and it has been found that during their oxidation the metal-ligand bond is broken to yield the free nitrilophenoxyl radical in solution which under the action of the transition metal salt undergoes cyclotrimerization with formation of the non-symmetrical triazine.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimiya, No. 5, pp. 1143–1146, May, 1984.     

Synthesis,crystal structures,and catalytic activities of palladium imidazole complexes formed by 2-hydroxyethyl group cleavage

N-4,6-dimethyl-2-pyrimidinylimidazole 1 and its hydroxyethyl derivative 1-(2-hydroxyethyl)-3-(4,6-dimethyl-2-pyrimidinyl)imidazolium chloride 2 have been synthesized and characterized. The attempted synthesis of bis(N-heterocyclic carbene)palladium complexes via the direct reaction of 2 with Pd(OAc)₂ results in the unexpected formation of a bis(N-arylimidazole) palladium complex 3. Additionally, the analogous bis(N-methylimidazole) palladium complex 4 has also been synthesized by the above method. Compounds 1–4 were characterized by elemental analysis, IR, and ¹H NMR. Additionally, their crystal structures have been determined by X-ray diffraction. Complexes 3 and 4 were found to be efficient catalysts for the Suzuki reaction.     

Synthesis of 3,5-dimethyladamantan-1-ol by reaction of 1,3-dimethyladamantane with bromotrichloromethane and water in the presence of manganese complexes

3,5-Dimethyladamantan-1-ol was synthesized in 79% yield by reaction of 1,3-dimethyladamantane with bromotrichloromethane and water in the presence of manganese salts and complexes activated by pyridine.     

The quasi-symmetric OHN and ODN bridges in the adducts of 3,5-dimethylpyridine with 3,5-dinitrobenzoic acid

The crystal structure of the adduct of 3,5-dimethylpyridine and 3,5-dinitrobenzoic acid (DMP-DNB) has been determined at room temperature and 80 K for both undeuterated and deuterated compounds. The monoclinic crystals are isomorphous, space group P2₁/c and Z = 4. Very strong OHN hydrogen bonds are almost linear with fully disordered (1:1) bridge hydrogen atoms between oxygen and nitrogen atoms. This is well reflected in the difference in electron density maps the contours of which depend both on cooling and deuteration. The intramolecular hydrogen bond lengths are 2.550(2) Å for the (OHN) and 2.563(2) Å for (ODN) at room temperature and 2.529(2) Å for (OHN) and 2.531(2) Å for (ODN) at 80 K. Therefore, there is a small but meaningful isotope effect upon the O…N hydrogen bridge length at room temperature and no Ubbelohde isotope effect is observed at 80 K. The infra-red spectra show very broad stretching protonic bands in the 200–1600 cm⁻¹ range. The isotopic ratio v(H)/v(D) at room temperature is about 1.1.     

Synthesis and structure of palladium triflates with coordinated 3,5-dimethylpyrazole

We discovered that reacting Pd₃(??-OOCMe)₃ with two moles of trifluoromethanesulfonic acid (Hotf) and then with four moles of 3,5-dimethylpyrazole (Hdmpz) in acetonitrile and benzene produces, in high yields, [Pd(Hdmpz)₄](otf)₂ and Pd(Hdmpz)₄(HOOCMe)₂(otf)₂, respectively. Reacting PhenPd(OOCMe)₂ with Hotf in MeCN yields PhenPd(NCMe)₂(otf)₂, where labile acetonitrile molecules are substituted by Hdmpz under mild conditions to form PhenPd(Hdmpz)₂(otf)₂. The structures of complexes have been solved on the basis of X-ray crystallography data.     

Synthesis of hydrocarbons from Co and H2 in the presence of supported Co catalysts modified by palladium

A study has been made of the effect of Pd on the activity and selectivity of Co catalysts prepared by impregnating various supports (SiO₂, SiO₂-Al₂O₃, Al₂O₃) with cobalt carbonyl or nitrate in the synthesis of hydrocarbons from CO and H₂. It is shown that the addition of Pd leads to an increase in the yield of liquid hydrocarbons and to a change in their composition. It has been established by IR spectroscopy that the introduction of Pd into the composition of carbonyl catalysts affects the formation of their surface.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 3, pp. 521–524, March, 1990.     

Reactions of aryl and heteryl iodides with terminal acetylenes in the presence of co,catalyzed by palladium complexes

The influence of the nature of the solvent, of the base, the catalyst, the temperature, and the pressure of CO on reactions of aryl and heteryl iodides RI with terminal acetylenes RCCH in the presence of CO, catalyzed by palladium complexes is studied.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 11, pp. 2548–2551, November, 1991.     

Alk-2-yn-1-amines in the synthesis of substituted quinolines in the presence of palladium complexes

An effective one-step procedure has been developed for the synthesis of 4- and 2,3,4-substituted quinolines via reaction of o-iodoaniline with alk-2-yn-1-amines in the presence of Pd(OAc)₂ as catalyst.