Synthesis of 2-trifluoromethyl-4,6-diphenyl-1,3,5-triazine

Conclusions Methods have been developed for the preparation of the simplest fluorine-containing phenyltriazine, viz., 2-trifluororaethyl-4,6-diphenyl-1,3,5-triazine, in virtually quantitative yield.Translated from Izvestiva Akademii Nauk SSSR, Seriya Khimieheskaya, No. 4, pp. 919–920, April, 1986.     

Synthesis of 2[(4,6-diphenyl-2H-pyran-2-ylidene)methyl]-4,6-diphenylpyrylium perchlorate

The title compound was prepared by the condensation of 4,6-diphenyl-2H-pyran-2-one and acetophenone in phosphorus oxychloride. The absorption spectrum of this 2,2-methine dye is compared with those of the corresponding 2,4- and 4,4-methine dyes.     

Reaction of 2,5-diphenyl-1,2,3-diazaarsole with 2-diazopropane

Conclusions The reaction of 2-diazopropane with 2,5-diphenyl-1,2,3-diazaarsole (I) gave 2,4-di-phenyl-6,6-dimethyl-1-arsa-2,3-diazabicyclo[3.1.0]hex-3-ene (III).Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 1, pp. 230–231, January, 1986.The authors thank R. M. Mukhamadeeva and P. N. Sobolev for taking the spectra.     

1-Methyl-3,5-diphenyl-4-aminopiperidin

Zusammenfassung 2,4-Diphenylacetessigester (I) lieferte, mit Methylamin-Formaldehyd und anschließend mit HCl behandelt, vermutlich über das Bispidinderivat II das 1-Methyl-3,5-diphenylpiperidon-(4) (IV) als Stereomerengemisch von Meso- (IV a) und Racemform (IV b). Das sowohl aus IV a wie aus IV b erhältliche Oxim VI gab bei der LiAlH₄-Reduktion ein 1-Methyl-3,5-diphenyl-4-aminopiperidin VII, dessen Konfiguration nicht ermittelt wurde.     

Preparation of fused meso-ionic compounds from 1-amino-4,6-diphenyl-2-pyridone

A number of meso-ionic compounds derivatives of the bicyclic system 1,3,4-oxadiazolo[3,2-a]pyridine have been prepared from 1-amino-4,6-diphenyl-2-pyridone, either by thermal way or $\text{via}$ iminophosphorane ($\text{4}$)     

X-ray diffraction study of 6-methyl-4,6-diphenyl-2-dicyano-methylene-1,2,5,6-tetrahydronicotinonitrile

It was demonstrated by x-ray diffraction analysis that 1-imino-5-methyl-3,5-diphenyl-2-cyclohexene-2,6,6-tricarbonitrile, which has been erroneously described in the literature as a 1-phenylethylidenemalononitrile dimer, actually has the 6-methyl-4,6-diphenyl-2-dicyanomethylene-1,2,5,6-tetrahydronicotinonitrile structure. The latter is one of three isomers that are formed as a result of the base-catalyzed dimerization of 1-phenylethylidenemalononitrile. The conformation of the unsaturated heteroring is discussed.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp. 71–74, January, 1988.     

5-Methyl-2-phenyl-2H-1,2,3-diazaarsole in reaction with ethyl diazoacetate

5-Methyl-2-phenyl-2H- 1,2,3-diazaarsole 1 reacts with ethyl diazoacetate to form a 1:1 bicyclic product 3a , 8-ethoxycarbonyl-4-methyl-2-phenyl-1-arsa-2,3,6,7-tetraazabicyclo[3.3.0]octa-3.7-diene. The latter isomerizes to a two-coordinate arsenic compound 5 , 3-ethoxycarbonyl-5-[α-(phenylhydrazono)ethyl] 1-1,2,4-diazaarsole. The X-ray crystal structure analyses of both products 3a and 5 have been carried out.     

Synthesis and alkylation of 4,6-diphenyl-3-thiocarbamoyl-3,4,5,6-tetrahydropyridine-2(1H)-one and 4,6-diphenyl-3-thiocarbamoyl-3,4-dihydropyridine-2(1H)-one

Alkylation of 3-thiocarbamoyl-3,4,5,6-tetrahydropyridine-2(1H)-one with methyl iodide has given 5-methylthio-2,6-diazabicyclo[2.2.2]oct-5-en-3-one and 3-methyl-thiocarbonyl-3,4-dihydropyridine-2(1H)-one. Alkylation of 3-thiocarbamoyl-3,4-dihydridine-2(1H)-one with iodoacetamide affords 3-(1-amino-1-carbamoyl-3,4-methyl-thiomethylene)-1,4-dihydropyridine-2-one, which in acidic media is converted into 3-(4-oxo-3,5-dihydro-1,3-thiazol-2-ylidene)-1,4-dihydropyridine-2-one.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 787–794, June, 1989.     

14N and 15N NMR Spectroscopy of 2-Methyl-4,5-dinitro-1,2,3-triazole and of Substituted 2-Methyl-4(5)-nitro-1,2,3-triazole 1-Oxides

Analysis of the ¹⁴N and ¹⁵N NMR spectroscopic data of 2-methyl-4,5-dinitro-1,2,3-triazole and of substituted 2-methyl-4(5)-nitro-1,2,3-triazole 1-oxides has shown the possibility of applying them for confirmation of the structures of the studied compounds.     

4-甲基-5-硝基-1,2,3-连三唑的合成

以丙二酸二乙酯为原料,经水解、硝化得到关键中间体偕二硝基乙酸乙酯(2);2与乙醛、叠氮化钠缩合环化得到4-甲基-5-硝基-1,2,3-连三唑(3)。3的结构经NMR,IR和元素分析表征。初步探讨了硝化反应的反应历程,并对制备2的合成进行了工艺改进,发现以NaNO2-98%HNO3为硝化试剂的新方法,2的收率达62.1%,纯度93.1%。     

2-乙酰基-5-甲基-1,2,3-二氮磷杂环戊二烯同丙炔醇反应研究

用付里叶变换红外光谱及³¹PNMR,探索了2-乙酰基-5-甲基-1,2,3-二氮磷杂环戊二烯同丙炔醇的动态反应过程,推测了可能的反应机理,并通过对二配位磷化物对应的三配位磷化物(2-乙酰基-3-氯-5-甲基-1,2,3-二氮磷杂环戊烯)同丙炔醇反应的研究,验证了二配位磷化物反应机理的可能性。     

Molecular structure of 1-dichloroacetyl-3,5-dimethyl-4,6-diphenyl-2-oxoperhydro-1,3-5-triazine

A. E. Arbuzov Institute of Organic and Physical Chemistry, Kazan Branch, Academy of Sciences of the USSR. Translated from Zhurnal Strukturnoi Khimii, Vol. 30, No. 5, pp. 189–192, September–October, 1989.