“…The (benzene-1,2-diselenolato)zirconocene and dipotassium benzene-1,2-diselenolate were obtained according to previously reported procedures. 12, 13 The (3-methoxybenzene-1,2-diselenolato)zirconocene 12 was prepared by literature methods. 14 The chloroethers used in the synthesis were commercial products, distilled before use.…”
Section: General Proceduresmentioning
confidence: 99%
“…The tetraselenacrown ethers 6-8 were prepared from the dihalogeno selenoethers 1-4 and dipotassium benzene-1,2-diseleno- late 5 according to Scheme 1. 6,12, 13 The reactions were performed using high dilution techniques and slow introduction of the reagents (pushed syringe). Following this strategy the yield increased with the length of the chain but remained quite low (10% for n = 1 and up to 25% for n = 3).…”
Section: Synthesis Of the Tetraselena Macrocyclesmentioning
confidence: 99%
“…Proton, 13 C and 77 Se NMR spectroscopic data for the crown ethers 6-8 and 14 are given in the Experimental section.…”
Section: Synthesis Of the Tetraselena Macrocyclesmentioning
“…The (benzene-1,2-diselenolato)zirconocene and dipotassium benzene-1,2-diselenolate were obtained according to previously reported procedures. 12, 13 The (3-methoxybenzene-1,2-diselenolato)zirconocene 12 was prepared by literature methods. 14 The chloroethers used in the synthesis were commercial products, distilled before use.…”
Section: General Proceduresmentioning
confidence: 99%
“…The tetraselenacrown ethers 6-8 were prepared from the dihalogeno selenoethers 1-4 and dipotassium benzene-1,2-diseleno- late 5 according to Scheme 1. 6,12, 13 The reactions were performed using high dilution techniques and slow introduction of the reagents (pushed syringe). Following this strategy the yield increased with the length of the chain but remained quite low (10% for n = 1 and up to 25% for n = 3).…”
Section: Synthesis Of the Tetraselena Macrocyclesmentioning
confidence: 99%
“…Proton, 13 C and 77 Se NMR spectroscopic data for the crown ethers 6-8 and 14 are given in the Experimental section.…”
Section: Synthesis Of the Tetraselena Macrocyclesmentioning
The para‐substituted diphenylzirconocenes [(t‐BuCp)2Zr(p‐C6H4R)2; R = Br, NMe2] (A) were easily obtained from the reaction of the appropriate organolithium reagent with bis(t‐butylcyclopentadienyl)zirconium dichloride. Elimination of bromobenzene or N,N‐dimethylaminobenzene from A by slight heating led to arynezirconocenes into which were inserted two equivalents of elementary chalcogens. As a result dichalcogenated zirconacycles [(t‐BuCp)2ZrY2C6H3R; Y = S, Se] (B) were obtained. Complexes B constitute useful potential synthons in organic synthesis and a large family of new functionalized dichalcogenated benzenic compounds was prepared by reacting electrophiles.
The structure of complexes B as well as related benzenic derivatives has been confirmed by microanalysis, 1H NMR and mass spectrometry.
288ChemInform Abstract The o-phenylenediselenobis(cyclopentadienyl)zirconium complex (I) reacts with the bifunctional electrophiles (II) to produce the benzodiselenaheterocycles (III), together with the zirconocenes (IV).
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