Dichloromethane, mass spectrum

Fig. 19.9. Electron ionization mass spectrum of dichloromethane (top panel) from GC-MS analysis, and library search match (bottom panel) against the NIST library.

The UV spectrum (Tmax 240, 268, 278, 288, 295, and 330 nm) of N-oxyellipticine (240) resembled that of ellipticine (228) (see Scheme 2.56), indicating a similar pyrido[4,3-l ]carbazole framework (222). Comparison of the mass spectrum of N-oxyellipticine at m/z 262 (M" ), with that of ellipticine (228) show only the presence of an additional oxygen as an N-oxy function. This conclusion was supported by comparison with the spectral data of synthetic Af-oxyellipticine, obtained by oxidation of ellipticine (228) with H2O2 in dichloromethane, and by reduction of Af-oxyellipticine with zinc to ellipticine. Based on these comparisons. 

In the mid 2000s, we initiated a comprehensive study of the coordination properties of orf/zo-phenylene bridged PBs. The DPB 8a was found to react with half an equivalent of [Rh2(g-Cl)2(nbd)2] in dichloromethane at room temperature (Scheme 62) 23 The yellow complex 108 that formed spontaneously was collected (92% yield) and analyzed spectroscopically. The 1H, 13C, and 31P NMR data substantiated the displacement of the labile nbd ligands at rhodium by the phosphine moieties. In addition, the mass spectrum indicated a dimeric structure of general formula [Rh2( i-C1)2(DPB2] and the nB NMR resonance signal observed at... 

AICI3 maintained at 170 °C. After 5 minutes, he poured the molten mixture into water and extracted it into dichloromethane. Evaporation of the dichloromethane gave a 96% yield of the product whose spectra follow. The mass spectrum of the product shows a molecular ion at m/z 132. What is the product ... 

The residue from dichloromethane extraction of hydrocracker deposits is a reddish powder. This material was found to be sparingly soluble in 1,2,4-trichlorobenzene (TCB). A mass spectrum of the TCB extract showed a major ion at 596 daltons, with peaks at 610, 624, and 638 daltons due to alkylation of this first species. Smaller peaks were seen at 620,... 

The phenylethynyl complex forms lemon-yellow crystals mp 205° (dec.) (checker, 200-205°), which are insoluble in light petroleum, diethyl ether, methanol, and ethanol but soluble in dichloromethane, chloroform, and tetra-hydrofuran. The infrared spectrum has a sharp v(C=C) band at 2068 cm"1, and the H nmr spectrum contains resonances at r 2.52m, 2.90m (35H, Ph) and 5.67s (5H, CSHS). The mass spectrum contains a parent ion centered on m/e 792 (calcd. for 102Ru, 792). 

The compound is stable toward air and moisture and is soluble in benzene, toluene, chloroform, and dichloromethane. On heating, the bright, black, diamagnetic crystals begin to decompose at about 195°. The structure of the complex has been established by a single-crystal X-ray determination.4 Its FD mass spectrum shows [M]+ at m/z 1034 (ref. to 98Mo32S). The 31P( H) spectrum of the... 

The 3-(r s-cyclopentadienyl)-l,2-dicarba-3-cobalta-ctoso-dodecaborane(l.l) is a yellow solid of mp 238-239°. The melting point is, however, dependent on the heating rate owing to easy isomerization. The mass spectrum of the compound exhibits a cut-off at m/z 258 and by TLC on Silufol silica gel sheet (see p. 234) with benzene as an eluant the compound shows an Rf value of 0.35. Two absorption bands in the electronic spectrum are recorded at 277 nm (e = 58,720) and 423 nm (e = 487) in dichloromethane as a solvent. The H-NMR spectrum in acetone-d6 shows a distinct signal of cyclopentadienyl protons at 5 5.87(5) and a broad C-H carbaborane signal at 4.49 ppm. The 1 B-NMR spectrum in the same solvent is composed of five doublets of relative intensities 1 1 4 2 1 cen-... 

Dichloromethane extracts and thermal desorption The chromatograms of the samples (Fig. 12) showed main peaks at 9.04, 11.61, 13.85, 17.45 and 17.87 min. Chlorodiphenylarsine (Clark I, 9.04 min), Triphenylarsine (11.61 min) and Bis(diphe-nylarsine)oxide (17.45 min, main degradation product of Clark I) could be identified using library searches. Bis(diphenylarsine) (17.87 min) has been identified by means of its mass spectra according to Schoene et al. (1995). Isotopic pattern calculation indicated the peak at retention times 13.85 min to contain sulfur. By comparison of the mass spectrum the substance could be identified as Diphenylthiophenylarsine as proposed by Schoene et al. (1995). 

The mass spectrum of unknown compound A shows a molecular ion at in/z 116 and prominent peaks at m/z 87 and ni/z 101. Its UV spectrum shows no maximum above 200 nm. The IR and NMR spectra of A follow. When A is washed with dilute aqueous acid, extracted into dichloromethane, and the solvent evaporated, it gives a product B. B shows a strong carbonyl signal at 1715 cm in the IR spectrum and a weak maximum at 274 nm (e = 16) in the UV spectrum. The mass spectrum of B shows a molecular ion of tn/z 72. 

Figure 8.53 Electron ionization mass spectrum of (a) bromobenzene and (b) dichloromethane.

Figure 5.8 (a) ESI mass spectrum in the positive ion mode of the reacting solution of trans-anethole (2) (0.5 mmol L ) and tris p-bromophenyl)aminium hexachloroantimonate (1) (5.0mmol L" ) in dichloromethane (reaction time approx. 7 seconds), (b) ESI-MS/MS of the ion of m/z 148 of the same reacting solution... 

In 1999, Che reported on the catalytic asymmetric amidation of the CH bonds of hydrocarbons by [(Porph )ML,L ] (M=Ru, L, L =CO, EtOH M=Mn, L=OH , MeOH Porph =l,2,3,4,5,6,7,8-octahydro-l,4 5,8-dimethyanoanthracen-9-yl) porphinato dianion) with PhINTs. The electrospray mass spectrum of a mixture of [(Porph )Mn(CO)(EtOH)] and PhINTs in dichloromethane displayed a significant signal for a PhINTs complex [(Porph )Mn(PhINTs)]. A Hammett-type study of substituted ethylbenzenes suggested, however, the reaction proceeded via ben-zylic radicals arising from H-atom abstraction by a manganese tosylamido intermediate [80]. 

Protonation of l,5-Fc2Aq with CF3SO3H in dichloromethane afforded a deep green precipitate, of which the ESl-mass spectrum indicated the formation of doubly protonated structure. Its UV-Vis-mear-IR absorption spectrum in Nujol muU, showing the transition characteristic of a ferrocenium ion = 766 nm) and... 

Treatment of 3 with wet acetonitrile at room temperature afforded the oxo-bridged dimer [(l,3-C5(Si(CH3)3)2H3)Ti(CF3C0CHCCX F3)(0)]2 (12, 73%, Scheme IV). T e same reaction occurred with diethyl ether or chloroform as solvent no intermediate hydrolysis products were observed. This is in contrast to the hydrolysis of 1, where 9 could be isolated and partially characterized. The structure of 12 was evident from the H and NMR spectra and from the mass spectrum, which showed a mass envelope corresponding to the parent ion of the dimer. Furthermore, the crystal structure was determined (31). Complex 12 could also be accessed in high yield by exposure of dichloromethane, chloroform, diethyl ether, or acetonitrile solutions of 10 to atmospheric moisture. Finally, hydrolysis of 12 in wet acetone (ca. 0.5% water) at room temperature afforded the tetrameric oxo complex 8 in 43% yield. 

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