Bis perchlorate

Addition of 2 mol equivalents of T " to alkynes gave bis-perchlorates 40 [R = H, Me, Ph R = R = MeO (geometry not established)], which were explosive upon heating. The alkyne reactions were much slower than those with alkenes, and no reaction at all occurred with ethyl propiolate, from which it was concluded that all these reactions have the character of electrophilic addition to the unsaturated unit (79JOC915). 

Xenon Perchlorate (Xenon (II) bis perchlorate), Xe(C104)2 mw 330.01 pale yel solid decompg to a red liq mp, detonates when heated over 20°. Sol in acetonitrile. Prepn is by treating Xe difluoride with 2 moles of anhydr perchloric add initially at —110°, and completing the reaction at -60°... 

This reaction of cyclohexene with (PhI + )20 2BF4 and lithium perchlorate gave exclusively the cz s-bis-perchlorate adduct (92%). Also, silyl enol ethers underwent efficient oxidative coupling to 1,4-diketones [24] ... 

Synthesis of 5,12-dimethyl-1,8-diaza-4,1 l-diazotetradeca-4,11-diene bis(perchlorate) (Scheme 1.16)... 

The synthesis of the octaethyl-substituted tetraoxa[22]porphyrin-(2.2.2.2) bis-perchlorate 4.162 has also been realized." This was accomplished via the McMurry-type reductive coupling of the ethyl-substituted diformyl-difuryldimethene 4.161 (Scheme 4.4.4). In this instance, however, the presumed non-aromatic intermediate was not isolated in pure form. Rather, oxidation with bis(trifluoroacet-oxy)iodobenzene followed by treatment with perchloric acid afforded the aromatic bisperchlorate salt 4.162 directly. 

C5 uH8oClaCui,Ni 2O22 / Bis(perchlorato)bis[ 1-(N,N-dimethyl-2-aminoeth-yl)-1-phenyl-2-oximatopropane]dicopper bis(methanol)bis[1-(N,N-di-methyl-2-aminoethyl)-1-phenyl-2 OXimatopropane]dicopper bis(perchlorate), 45B, 1051... 

Cl8H28CI2C0N4O10 f Diaquo(2,3,9,1O-tetramethyl-1,4,8,11-tetraazacyc-lotetradeca-1,3,8,10-tetraene)cobalt(II) bis(perchlorate), 43B,... 

C31H27BM0N9O2P, Tetrakis<1-pyrazolyl)borato(triphenylphosphine)(carbonyl) (nitrosy1)molybdenum, 43B, 1331 C3 2H2 nCdCl2N808, Tetrakis(1,8-naphthyridine)cadmium(11) bis(perchlorate), 40B, 915... 

C2iiHi,6Cl2Ni,Oi5, Aquatetrakis(N-f ormylpiperidine)dioxouranium(VI) bis(perchlorate), 46B, 1156... 

An interesting D-ring closure was used by Pakrashi and his coworkers to synthesize normalindine (466) and norisomalindine (467) (Scheme 3.81) (130). Imine 462, prepared by condensation of tryptamine and 3-acetylpyridine, was reduced and the formed amine was acetylated to afford amide 463. Bischler-Napieralski cyclization of 463 provided tetracyclic iminium bis-perchlorate salt 464 which when treated with triethylamine and pivaloyl chloride underwent a second cyclization to yield the pentacyclic enamine 465. Reduction of the olefinic group in 465 afforded the desired azayohimbines, 466 and 467. 

Koleva, B.B., T. Kolev, T. Tsanev, St. Kotov, H. Mayer-Figge, R.W. Seidel, and W.S. Sheldrick. 2008. Crystal stmcture, optical and magnetic properties of the bis(perchlorate) of 3,4-diaminopyridine. Sfracf. Chem. 19 13-20. 

---