A series of novel C60 rhodium complexes [Rh(acac)(L)2(η2-C60)] (L = pyridine, 4-methylpyridine, 3,5-dimethylpyridine) were prepared by the reaction of [Rh(acac)(C2H4)2] with C60 followed by treatment with pyridine or its derivatives. The molecular structure of [Rh(acac)(3,5-Me2py)2(η2-C60)]·C6H6 was determined by the X-ray crystallographic analysis.
C2oH24NO5P, Mr=389"40, monoclinic, P2~/a, a = 15.332 (3), b = 10-603 (6), 3 c= 12.442 (6) ,h,, fl = 100.89 (3) °, V = 1986 (1) A, Z = 4, Dx=l.30gcm -3, MoKa, A=0"7107A, /z = 1.84cm -~, F(000)= 824, room temperature, R= 0.059 for 2108 observed reflections [Fo > 3or(Fo)]. Out of l l C---C bonds of the biphenyl ring, four bonds (1-35-1-38 A) are significantly shorter than the others * Present address: (1-40-1.43 A). Two P--O single bonds are 1.564 (4) and 1-560 (4)/~ in length, and the P--O double-bond length is 1-454 (4) A. Experimental. Title compound prepared according to the literature (Takeuchi, Shibata & Hamada, 1984). Colorless crystals obtained from ethanol solution. Crystal of dimensions 0.3 × 0-2 × 0.2 mm, Rigaku AFC-1 rotating-anode four-circle diffractometer, graphite-monochromatized Mo Ka radiation. Cell dimensions determined from 16 20 angles in the range 17 < 20 < 23 °. Intensities collected to sin0/a =
The rate constants of the thermal dissociation of carbaminic acid esters in fatty acids were determined. In the case of phenylcarbaminic acid alkylestees, the rates showed the following order. tert-Bu>>isoPr≥Me
The relative rates may be considered to denote the ability of —OR groups as proton acceptors and the results of the experiment can be explained by the inductive effect of the substituted alkyl-groups.
In the case of alkylcarbaminic acid phenyl-esters, the rates showed the following order. Acetyl>>isoPr>Me
The relative rates may be considered to denote the ability of (Remark: Graphics omitted.) groups as proton donors. In acetylcarbaminic acid phenylester, because of the resonance effect of the (Remark: Graphics omitted.) and COOR groups, the intervening nitrogen aquires a positive potential. The phenomenon will make the hydrogen attached to nitrogen have more tendency to transfer, hence the reaction. That isopropylcarbaminic acid phenylester dissociates faster than methyl-carbaminic acid phenylester will be explained by the steric effect of alkyl-groups.
The rates of the thermal dissociation of esters depend on the nature of the solvent acids.
Faculty, University of Meijo*2) 1) Condensation of (III) with ammonia, dimethylamine, piperidine, aniline, paniline, and 2, 4-dichloroaniline in ethanol gave the compounds (IV to IX) which were reduced to (X to XII), and acetylated to (XIII to XV). Application of phenol, p-nitro phenol, and p-cresol to (III) gave the compounds (XVI to XVII). Similar condensation of 4, 8-dichloroquinaldine with aniline, p-chloroaniline, p-nitroaniline, and anisidine in ethanol gave the compounds (XIX to XXII). 2) Similar condensation of 2-chlorolepidine or 2-chloro-5-nitrolepidine with pchloroaniline, p-nitroaniline, and p-anisidine gave (XXIII to XXV) and (XXVI to XXVII). The compound (XXIX), obtained by nitration of 2-hydroxylepidine followed by chlori nation, was identified with 2-chloro-6-nitrolepidine. Similar condensation of (XXIX) and 2-chloro-8-nitrolepidine with p-aminoaniline, p-chloroaniline, and p-anisidine gave the compounds (XXX to XXXV). These compounds were submitted to antifungal test with Candida.
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