This r eport describes th e sy nt hesis of a new bis-bifunctional derivative of 8-hyd ro xyquinolin e, its reaction with a number of divalent, first-row trans it ion m etals to form coo rdin ation polymers, and a t hermogravimetric study of the thermal stabili ty of the polyme rs. The ligand, 5,5'-[methylenebis (p-phenylenen it rilometh ylid yne) ]di-8-quinolinol was prepared in a condensation r eaction between 5-formyl-8-hyd rox yq uin oline a nd 4,4'-meth yle nedianiline and subsequently treated with t he acetate salts of Mn(II) , Co(I1), N i(II), eu(II), and Zn (II). Th e metal coo rdi nated in t he backbone of t he polymer is sh own to be an important factor in gove rning the thermal stability w hen t he sampl es a re heated in vacuum.
A condensation reaction between 5amino-%hydroxyquinoline and terephthalaldehyde yielded a bis-bifunotional Schiff base ligand, 5,5'-[pphenylene-bis(methy1i-dynenitrilo)] di-%quinoliioi, which was used to produce coordination polymers containing Mn(II), Co(II), NYII), Cu(II), or Zn(I1) in the form of insoluble powders. The thermal stabilities of these polymers were evaluated in vacuum over the temperature range of 25-700°C. by using a newly constructed thermobalance having improved sensitivity. The results relate the decomposition of the polymers to the metal in the backbone aa well 88 to the organic ligand to which the metal is coordinated. Some discussion is devoted to the possible modes of decomposition of these polymers.
The tetrahydrofuran layer was separated and evaporated in vacuo to an oil. This oil was fractionally distilled, dissolved in abs. ether and dried over sodium hydroxide pellets. The pure hydrazine was obtained by fractionally distilling this ether solution.N-Nitrosomethylaniline was reduced to 1-methyl-l-phen-ylhydrazine5 in 77% yield which is an oil boiling at 106-109°( 13 mm.).N-Nitrosopiperidine was reduced to N,N-pentamethylenehydrazine* in 75% yield. It is an oil boiling at 146-148°( 730 mm.).N-Nitrosodicyclohexylamine was reduced to 1,1-dicyclohexylhydrazine in 48% yield. It is a white crystalline solid boiling at 95-98°( 4 mm.) which sublimes above 162°. The hydrochloride forms white flaky crystals from ether, m.p. 238-240°( cor.). The methiodide forms small white plates from abs.
In spite of the experimental failures to prepare praseodymium tetrafluoride, there is strong evidence for its possible formation to be found by calculating the equilibrium constants for some of the reactions by which this compound might be prepared.
Ion in Aqueous Solution 1301 is a difficult one, especially if only the powder pattern is available and if the compound contains heavy uranium as well as light oxygen, silicon, and hydrogen atoms.Data and Discussion.-Analytical samples were limited to 0.100 g. since only a small over-all amount of compound was available. The analytical accuracy of approximately ±0.3% for uranium is much better than was attained for silicon or for water due to the very large atomic weight of uranium. Therefore, greater reliance should be placed on the uranium analyses.
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