2-甲基-4-羟基-6-苯基嘧啶和2-甲基-4-羟基-5-溴-6-苯基嘧啶的高效液相色谱法分离测定

采用ODS-C18色谱柱和紫外检测器,对2-甲基-4-羟基-6-苯基嘧啶和2-甲基-4-羟基-5-溴-6-苯基嘧啶的含量进行HPLC分离测定.以甲醇水=4555为流动相,紫外检测波长为237 nm,样品线性范围为0.001～0.1 mg/mL.2-甲基-4-羟基-6-苯基嘧啶的RSD为0.5%;2-甲基-4-羟基-5-溴-6-苯基嘧啶的RSD为1.0%.     

Reactions of 2-Amino-4-methyl-6-(2-pyridyl)- and 2-Amino-4-methyl-6-phenyl-7,8-dihydroindazolo[4,5-d]thiazoles with Aldehydes

The reaction of 2-amino-4-methyl-6-(2-pyridyl)-7,8-dihydroindazolo[4,5-d]thiazole, obtained by treating 3-methyl-4-oxo-1-(2-pyridyl)-4,5,6,7-tetrahydroindazole with pyridinium bromide perbromide and then with thiourea, and 2-amino-4-methyl-6-phenyl-7,8-dihydroindazolo[4,5-d]thiazole with 4-bromo-, 4-fluoro-, 4-dimethylamino-, 4-methoxy-, 3,4-dimethoxy-, and 3,4-methylenedioxybenzaldehydes, furfural, pyridinecarbaldehyde, and thiophenecarbaldehyde gave the corresponding Schiff bases. The products of the condensation of these aminothiazoles with cinnamaldehyde, 1-(2-pyridyl)- and 4-chloro-1-(2,4-difluorophenyl)-5-formyl-3-methyl-6,7-dihydroindazoles, 2-formyl-dimedone, and 2-formyl-1,3-indanedione were also obtained.     

Synthesis starting from 3-methyl-2-phenyl-5-(3-methyl-2-phenyl-3,4-dehydropiperidyl-6)pyridine. 2-phenyldinicotinic and 4-azafluorenone-2-carboxylic acids

N-Methyl (ethyl, benzoyl, trifluoroacetyl)-substituted 3-methyl-2-phenyl-5-(3-methyl-2-phenyl-3,4-dehydropiperidyl-6) pyridines and di(N-oxide) of the correspondingly substituted ,ß-dipyridyl were prepared. A method for synthesizing 2-phenyldinicotinic acid was developed. Cyclodehydration of this acid gave 4-azafluorenone-2-carboxylic acid. Transformations of this acid were carried out with respect to two functional groups.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 813–817, June, 1986.     

Some properties of α-(6-methyl-2-benzothiazolyl)α-phenyl-β-picrylhydrazyl, α-(2-methyl- 6-benzothiazolyl)-α-phenyl-β-picrylhydrazyl,and their hydrazines

The structures and properties of -(6-methyl-2-benzothiazolyl)--phenyl--picrylhydrazyl, -(2-methyl-6-benzothiazolyl)--phenyl--picrylhydrazyl, and their corresponding hydrazines nd complexes were studied by means of IR, UV, and visible spectroscopy and electrical conductivity. The half-wave potentials and limiting currents for reduction on a dropping mercury electrode were found for the hydrazines. The charge and spin densities of the investigated compounds were calculated by the Hückel MO and MacLachlan methods. It is shown that in the case of strong interaction with a medium the characteristics of the trinitrophenyl groups of the picrylhydrazines are practically the same, regardless of the structure of the hydrazine residue bonded to them.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 462–467, April, 1971.     

Synthesis and properties of 1-methyl-2-phenyl-5-(2-furyl)- and 1-methyl-2-phenyl-5-(2-thienyl)imidazoles

2-Phenyl-5-(2-furyl)- and 2-phenyl-5-(2-thienyl)imidazoles were synthesized by condensation of 2-furoylmethyl and 2-thenoylmethyl acetates with benzaldehyde under the conditions of Weidenhagen reaction. The products were converted to N-methyl derivatives in the KOH-acetone system. The electrophilic substitution reactions of the products (acylation, bromination, nitration, sulfonation, hydroxymethylation) were studied.     

NMR parameters,isomerism, and conformational analysis of 3-methyl-2-phenyl-5-(3-methyl-2-phenyl-3,4-dehydropiperid-6-yl)-pyridine

The configurational and conformational features of the trans and cis isomers of 3-methyl-2-phenyl-5-(3-methyl-2-phenyl-3,4-dehydropiperid-6-yl)pyridine, formed as by-products in the phenylation of -picoline by phenyllithium, were established. The revealed stereospecificity of the ⁵J_HH and ¹J_CH SSCCs may be utilized as an independent criterion in the conformational analysis of piperideine systems.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp. 71–74, January, 1993.     

Synthesis and investigation of the properties of α-(6-methyl-2-benzothiazolyl)-α-phenyl-β-(2,6-dinitrophenyl)hydrazyl, α-(2-methyl-6-benzothiazolyl)-α-phenyl-β-(2,6-dinitrophenyl)-hydrazyl,and the correspondinghydrazines

-(6-Methyl-2-benzothiazolyl)--phenyl--(2,6-dinitrophenyl)hydrazyl and -(2-methyl-6-benzothiazolyl)--phenyl--(2,6-dinitrophenyl)hydrazyl and their corresponding hydrazines were synthesized. The properties of the compounds obtained were investigated by IR, UV, and visible spectroscopy. Their complexing ability was studied by an optical method and from their electrical conductivity. The ESR spectra of the radicals were recorded. The limiting currents and reduction potentials of the hydrazines on a dropping mercury electrode were found. The charge and spin densities of the compounds were calculated by means of the Hückel MO and MacLachlan methods. It was demonstrated that the hydrazines form unstable charge-transfer complexes in benzene—piperidine solutions; the characteristics of these complexes depend on the structure of the RRN-NH-hydrazine residue.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 11, pp. 1484–1490, November, 1971.