Improved Synthesis of 1-Aryl-2, 2-Dichloro-1-Alkanones

Recently¹ we described a convenient synthesis of 1-aryl-2, 2-dichloro-1-alkanones 1 by a reaction sequence involving conversion of the parent alkylarylketones into the corresponding N-cyclohexylketimines, followed by chlorination with N-chlorosuccinimide in carbon tetrachloride to afford N-cyclo-hexyl α,α-dichloroketimines, the latter compounds being hydrolyzed in acidic medium to yield the title compounds 1. The relative inaccessibility of compounds of type 1 in the literature was striking. α,α-Dichloroacetophenones 1 (R=H) are     

4-氨基-3,5-二氯-2′-溴苯乙酮的合成研究

溴化铜的溴代反应结果表明：在反应温度为６０℃,原料的摩尔配比为４－氨基－３,５－二氯苯乙酮∶溴化铜＝１∶２,反应２．２ｈ合成标题化合物,溴代产率可达９５％以上     

1,3-二氯-1,1′,3,3′-四(1,3-二苯基-1,3-丙二酮)-μ-氧合钛(Ⅳ)的晶体结构与分子结构

本文报导了氧桥双核钛配合物[TiCl(BZBZ)_2]_2O的晶体结构和分子结构。配合物晶体(分子式C_(60)H_(44)Cl_2O_9Ti_2)属单斜晶系,C2/c空间群,a=21.013(7),b=18.509(2),c=17.493(2),β=91.43(2)°,V=6801.5(?)~3,M_r=1075.72,Z=4,D_x=1.05 gcm~(-3),μ=3.54 cm~(-1),F(000)=2216,R=0.104(1887个可观测衍射)。配合物分子由Ti—O—Ti桥氧骨架构成,有一分子内二重轴通过桥氧原子。对配合物的生成机理作了探讨。     

Synthesis of Some New Derivatives of 1,3-Dichloro-1,1,3, 3-tetraphenyldisilazane

Recently, the silicon-nitrogen compounds have received more consideration for their attractive application prospects. Both low molecular weight silazane and polysilazane with high molecular weight are widely used in many aspects. For example, in the processing industry of silicone rubber, silizanes not only can be used as "structure-control additives"1, but also can be used to improve the rubber's heat-resistance and mechanical properties; silicon-nitride ceramics can be prepared by pyrolysis …     

Triphenylphosphine-Catalyzed Synthesis of Stable,Functionalized 2H-Oxetes

Triphenylphosphine underwent Michael addition to dialkyl acetylenedicarboxylate and subsequently to the carbonyl group of α-haloketones. Then, these compounds were cyclized to produce the unstable 1, 3-diionicphosphorus compound, which spontaneously lost triphenyl phosphine, and was converted to the functionalized oxetes derivatives.     

Synthesis and Phosphorylation of 2- and 3-Halomethyl Derivatives of Functionalized 2-tert-Butylfurans

2-Halomethyl derivatives of 3-functionalized 5-tert-butylfurans are phosphorylated underconditions of the Michaelis-Becker, Arbuzov reactions similarly to other halomethylfurans. No effectof the tert-butyl substituent on the yield of the reaction products was found in this case. Contrary to that, the2-methoxymethyl derivative of 3-chloromethyl-5-tert-butylfuran proved to be more thermostable than its analog containing no tert-butyl substituent. As a result, the yield of phosphonate in the Michaelis-Becker reaction under similar conditions increases 2.5 times. The observed stabilization of the furan ring is explained by shielding of its oxygen atom by the tert-butyl group.     

Synthesis and Crystal Structure of (3,6-Dichloro-2-nitrophenyl)(3-nitrophenyl)methanone

Novel compounds, (3,6-dichloro-2-nitrophenyl)(3-nitrophenyl)methanone(2), (2-amino-3,6-dichloro- phenyl)(3-aminophenyl)methanone(3) and 1-[3-(2-amino-3,6-dichlorobenzoyl)phenyl]-1H-pyrrole-2,5-dione(4), were synthesized from the initial compound 2,5-dichlorobenzophenone(1) and characterized by 1H NMR, 13C NMR, IR, mass spectrum and element analysis, respectively. The single crystal of compound 2 was obtained and determined by X-ray diffraction analysis. The single crystal data illustrates that it belongs to...     

A Practical Synthesis of 2,4-Dichloro-3-methyl-6-nitrophenol

2,4-Dichloro-3-methyl-6-nitrophenol 2 was prepared by KOH/H₂O hydrolysis of a product mixture obtained from chlorination of p-nitrotoluene in the presence of a phase transfer catalyst. A 95–99% yield of 2 based on 2,3,6-trichloro-4-nitrotoluene, 4 (major chlorination product) was achieved in >95% purity.     

阻燃中间体3,9-二氯-2,4,8,10-四氧代-3,9-二磷杂螺[5.5]十一烷的合成

以PCl3和季戊四醇为原料合成了中间体3,9$C二氯-2,4,8,10$C四氧代-3,9-二磷杂螺[5.5]十一烷,产率达99.6%.对反应条件进行了优化,最佳反应条件为:PCl3和季戊四醇摩尔比为2.5∶1,反应温度80℃,反应时间1.5h.     

Synthesis and properties Of 1-vinyl-2, 2, 3, 3-tetrafluorocyclobutane

The oxidation, hydrobromination, and bromoacetylation of 1-vinyl-2, 2, 3, 3-tetrafluorocyclobutane are investigated, with a view to preparing its oxide. It is found that the most convenient method of preparing this oxide is acetyl hydroperoxide oxidation of 1-vinyl-2, 2, 3, 3-tetrafluorocyclobutane.The authors wish to thank V. A. Klimova and N. V. Korshun for elementary analyses, and B. V. Lopatina and L. V. Orlova for spectroscopic analyses of the compounds prepared.     

Synthesis of Highly Functionalized 1-Azadienes and Ketenimines

Summary. The 1:1 reactive intermediate generated by the addition of alkyl isocyanides to dialkyl acetylenedicarboxylates was trapped by fairly strong NH-acids such as carbazole, indole, or pyrrole to yield highly functionalized 1-azadienes and ketenimines.     

Synthesis of Highly Functionalized 1-Azadienes and Ketenimines

The 1:1 reactive intermediate generated by the addition of alkyl isocyanides to dialkyl acetylenedicarboxylates was trapped by fairly strong NH-acids such as carbazole, indole, or pyrrole to yield highly functionalized 1-azadienes and ketenimines.     

KI-Mediated Chlorine Gas-Free Synthesis of 3,3-Dichloro-2-oxindole Derivatives

An efficient and environmentally friendly methodology for 3,3-dichlorination and 2-oxidation of indole derivatives is described. Using KI as promotor, MCl (M=K, Na) as chlorine source, and oxone as oxidant, the reaction proceeds smoothly affording various functionalized 3,3-dichloro-2-oxindoles in moderate to excellent yields. This strategy can also be extended to 3-substituted indoles. With a broad substrate scope, it is a practical approach to 3,3-disubstituted-2-oxindoles.     

Some Novel Quinone-Type Compounds Containing Arylseleno Groups Derived from Tetrachloro-1, 4-Benzoquinone and 2, 3-Dichloro-1, 4-Naphthoquinone

Tetrachloro-1, 2-benzoquinone and 2, 3-dichloro-1, 4-naphthoquinone react with a series of aryl and alkyl selenolate, generated either by the reaction of Grignard reagents and selenium powder or by the reduction of diselenides with NaBH₄, to give 3, 6-diarylseleno-2, 5-dichloro-1, 4-benzoquinones 3 and 2, 3-diarylseleno-1, 4-naphthoquinones 4 in good yields.     

Synthesis of Functionalized Bicyclic Compounds Based on 2-(1-Arylethylidene)malononitriles

Russian Journal of Organic Chemistry - New tetrahydroisoquinoline-5,7-dicarbonitrile derivatives have been synthesized by piperazine hydrate-catalyzed reaction of acetoacetanilide with...     

Synthesis of New Highly Functionalized 1H-Indole-2-carbonitriles via Cross-Coupling Reactions

An approach for the preparation of polysubstituted indole-2-carbonitriles through a cross-coupling reaction of compounds 1-(but-2-ynyl)-1H-indole-2-carbonitriles and 1-benzyl-3-iodo-1H-indole-2-carbonitriles is described. The reactivity of indole derivatives with iodine at position 3 was studied using cross-coupling reactions. The Sonogashira, Suzuki–Miyaura, Stille and Heck cross-couplings afforded a variety of di-, tri- and tetra-substituted indole-2-carbonitriles.     

Efficient Synthesis of Highly Functionalized,S -Alkyl 1-Alkyl-4,4-dimethyl-2,5-dioxo-pyrrolidine-3-carbothioates

5-Isopropylidene-2,2-dimethyl-1,3-dioxane-4,6-dione (the condensation product of Meldrum's acid and acetone) reacts with alkyl isocyanides in the presence of this to produce S -alkyl 1-alkyl-4,4-dimethyl-2,5-dioxo-pyridine-3-carbothioates in good yield.     

Synthesis of Substituted 4-Arylsulfonylaminothiazoles from N-(2,2-Dichloro-2-phenyl-1-thioacetylaminoethyl)arenesulfonamides

Russian Journal of Organic Chemistry -     

Synthesis and reactions of 2, 3-dichlorothianaphthene-1-oxide

Oxidation of 2, 3-dichlorothianaphthene affords 2,3-dichlorothianaphthene-1-oxide. This reacts with methanol, ethanol, and piperidine to give 2-chloro-3-methoxy-, 2-chloro-3-ethoxy-, 2, 3-diethoxy-, and 2-chloro-3-piperidinothianaphthene-1-oxide.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 9, pp. 1192–1193, September, 1970.     

Synthesis of Functionalized Heterocycles on the Basis of 2H-1,2,3-Diazaphospholes

Abstract

The reactions of the cyclic derivatives of the two-coordinated phosphorus atom - 2-phenyl- and 2 -acetyl-2-H-l,2,3-diazaphospholes, dialkylphosphoe sulphenyklorides, dialkyldithio- and dialkylmonothiophosphates kads to the formation of the new P(III)-fUnctiohalized diazaphosphoknes.