Binary and ternary complexes of copper(II) with some dihydroxycoumarins

The complexation behaviour of copper(II) with a series of selected dihydroxycoumarins has been studied. Copper(II) binary complexes with esculetin, daphnetin and their 4-methyl and 4-phenyl derivatives and ternary complexes having a secondary ligand, ammonia or pyridine have bean synthesized. The general composition of binary complexes has bean found to be [Cu (H₂O)₂ (HL)₂] and that of ternary complexes as [Cu (L) (X)₄] (where X = NH₃ or C₅H₅N). The magnetic studies indicate all the complexes to be monomeric in nature. IR studies show that one of the two phenolic hydroxyl groups present in the ligand is lost during complexation. It is concluded that of the four ligands attached to the copper atom dihydroxycoumarin is bound most firmly.     

The synthesis of some 7- and 7,8-substituted 2,3,4,5-tetrahydro-1H-3-benzazepines

The nitration of 2,3,4,5-tetrahydro-1H-3-benzazepine and its 3-methyl and 3-acetyl derivatives yields the corresponding 7-nitro derivatives which can be further transformed by classical procedures. The preparation of the ether cleavage products of the known 2,3,4,5-tetrahydro-7,8-dimethoxy-1H-3-benzazepine is also reported.     

1-(2-pyridyl)-3,4-dihydro-6,7-dimethoxyisoquinoline and some of its hydrogenated and N-substituted derivatives

The preparation of 1-(2-pyridyl)- and 1-(2-piperidyl)-substituted, partly hydrogenated derivatives of 6,7-dimethoxyisoquinoline is described.     

Imidazoindoles. 3. Alkylation of 7,8-dimethylimidazo[4,5-e] indole

It is demonstrated that products of monoalkylation of 7,8-dimethylimidazo[4,5-e]-indole at the N₃ atom are formed in dioxane in the presence of sodium alkoxide or an aqueous solution of potassium hydroxide in the case of alkylation with alkyl halides, ethylene oxide, and acrylonitrile. The structures were proved by alternative synthesis and comparison of the UV spectra with the spectra of model structures.See [1] for Communication 2.Deceased.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1369–1373, October, 1980.     

Alkylation of nido-7,8-Dicarbollide Anion with Propargyl Bromide in Liquid Ammonia with Formation of 8-Propargyl-nido-7,9-dicarbaundecaborate and 9-Propargyl-nido-7,8-dicarbaundecaborate Anions

Alkylation of nido-7,8-dicarbollide anion with propargyl bromide in liquid ammonia is accom panied by skeleton rearrangements and yields, depending on the reaction conditions, 8-propargyl-nido-7,9-dicarbaundecaborate or 9-propargyl-nido-7,8-dicarbaundecaborate anion.     

Synthesis of some N-methylated pteridines related to 7,8-dihydroxanthopterin

Seven methylated pteridines have been synthesized by condensation of a 4-chloro-5-nitropyrimidine with a β-ketoamine (or a blocked derivative), reduction of the nitro group, and subsequent ring closure. This scheme provides a new route to dihydroxanthopterin. Several cases are reported, however, in the uracil series where ring closure could not be effected.     

7,8-二氢-6,6-二甲基-7,8-环氧-6氢-吡喃[2,3-f]苯并-2,1,3-噁二唑的合成

本文给出了一条较好的制备7,8-二氢-6,6-二甲基-7,8环氧-6氢-吡喃[2,3-f]苯并-2,1,3-噁二唑的合成路线,即由对乙酰氨基苯酚经酯化、Fries重排、环合、还原、脱水、硝化、脱酰基、氧化、脱氧和催化环氧化等反应制得标题化合物,其结构经元素分析和光谱数据确证。     

Oxa-Pictet-Spengler reaction in water. Synthesis of some (±)-1-aryl-6,7-dimethoxyisochromans

An acid catalyzed oxa-Pictet-Spengler reaction ‘on water’ leading to the synthesis of a variety of 1-aryl-6,7-dimethoxyisochromans is described. The aqueous chemistry is a much cleaner, efficient, cheaper and simple method for synthesis. The scope of reactions was extended to thia-Pictet-Spengler reaction to afford the some isothiochromans.     

Synthesis of some N-substituted 6,7-dimethoxy-1,2-benzothiazin(4H)-3-one 1,1-dioxides

Substituted 1,2-benzothiazin-3-ones have been prepared by cyclization of 4,5-dimethoxy-2-carboethoxymethybenzenesulfonamides. The latter were obtained by the action of ammonia and primary and secondary amines on 4,5-dimethoxy-2-carboethoxymethylbenzenesulfonyl chloride which in turn was obtained from ethyl 3,4-dimethoxyphenylacetate and chlorosulfonic acid.     

(S)-(+)-6,7-丙酮缩二醇-3-酮-庚酸乙酯的合成研究

首次报道利用丙二酸亚异丙酯钠盐与γ-丁内酯类化合物反应,制备β-酮酯类衍生物。以(S)-(+)-谷氨酸为起始物经重氮化、环合,加成开环及酯化等反应,成功地合成了(S)-(+)-6,7-丙酮缩二醇-3-酮-庚酸乙酯。化合物(1)、(5)、(6)未见文献报道。     

Synthesis of unsaturated 7,8- and 7,9-di(hydroxymethyl)decahydro-7,8- and-7,9-dicarba-nido-undecaborate(1−) diethers

Dicarba-nido-undecaborate(1–) anions were obtained by treatment of 1,2-di(hydroxymethyl)-1,2-dicarba-closo-dodecaborane(12) diallyl ether, 1,2-di(hydroxymethyl)-1,2-dicarba-closo-dodecaborane (12), and 1,7-di(hydroxymethyl)-1,7-dicarba-closo-dodecaborane(12) with ethanolic solutions of KOH and subsequent reaction of the products with cesium and tetramethylammonium chlorides.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1821–1823, September, 1995.     

(±)-6,7-丙酮缩二醇-3-酮-庚酸乙酯合成研究

用对甲苯磺酸-2,3-丙酮缩甘油酯(2)与乙酰乙酸乙酯盐、碳酸二乙酯反应, 制备β-酮酯类衍生物1. 以(±)-1,2-丙酮缩甘油为起始物, 经对甲苯磺酰化、亲核取代、脱羧等反应, 方便、高产率地合成了6,7-丙酮缩二醇-3-酮-庚酸乙酯(1). 试图通过对甲苯磺酸-2,3-丙酮缩甘油酯(2)和乙酰乙酸乙酯双阴离子反应制备6,7-丙酮缩二醇-3-酮-庚酸乙酯(1)未获成功. 所合成的化合物经元素分析, IR, ¹H NMR, ¹³C NMR和MS光谱表征.     

Synthesis of 6,7-Dihydroindazole and 7,8-Dihydroquinazoline Derivatives from Ethyl 4,4-Dimethyl-9-oxo-3,4-dihydro-9H-xanthene-2-carboxylates

Russian Journal of General Chemistry - A procedure has been developed for the synthesis of 6,7-dihydroindazoles and 7,8-dihydroquinazolines by reaction of 3,4-dihydroxanthone derivatives with 1,2-...     

Alkylation of some 6-substituted purines under interphase catalysis conditions

The mixture of 9-, 3-, and 7-benzyl-6-substituted purines is formed in almost quantitative yield by the alkylation of 6-benzylamino-, 6-furfurylamino-, 6-methylthio-, and 6-chloropurine with benzyl halides in the biphasic system of the liquid-liquid or liquid-solid type in the presence of interphase catalysts (quaternary ammonium salts, 18-crown-6). The catalytic activity of the quaternary ammonium salts increases with the increase in the lipophilicity of the cation. Taking the alkylation of 6-benzylaminopurine as an example, the possibility of the application of triphasic catalysis in the alkylation reaction of purines is indicated. The alkylation of 6-substituted purines with isopropyl bromide proceeds regioselectively under the conditions of the interphase catalysis with the formation of the corresponding 9-isopropylpurines.For the preliminary communication, see [1].Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp. 113–118, January, 1987.     

Synthesis and polymerizability of 7,8-dicyano-7,8-diphenylquinodimethane

7,8-Dicyano-7,8-diphenylquinodimethane (DCDPQ) was prepared by oxidation of the dianion of α,α′-dicyano-α,α′-diphenylxylene. ¹H-NMR of a solution of the purified compound showed that the cis and trans isomers were present in a 1:1 ratio. Following further spectroscopic and electronic characterization the polymerizability of the title compound was investigated. DCDPQ did not homopolymerize at 65°C in the presence of AIBN. DCDPQ copolymerized with p-methoxystyrene and p-aminostyrene in the presence of AIBN at 65°C. Characterization of the latter two copolymers indicated that they were nearly alternating. The copolymerization between DCDPQ and p-aminostyrene proceeded in the absence of AIBN.     

The Improved Preparation of 7,8-Dihydro-Quinoline-5(6H)-One and 6,7-Dihydro-5H-1-Pyrindin-5-one

Compounds 7,8-dihydroquinoline-5(6H)-one (3) and 6,7-dihydro-5H-1-pyrindin-5-one (5) are formed by new methods from 1,3-diketone compound, ammonium acetate and 1,1,3,3-tetraethoxylpropane.