Methanol proton magnetic resonance spectrum

A short-path distillation apparatus is used, the distillate (oxa-spiropentane plus dichloromethane) being trapped in a reeeiver placed in a methanol-dry ice bath cooled to — 80°. The checkers found it useful to drive out last traces of product by adding several milliliters of dichloromethane to the residual thick paste and distilling. The proton magnetic resonance spectrum (dichloromethane) shows an oetet at 8 0.85 and a singlet at S 3.00 in the ratio 4 2. 

The a-plienylcinnamonitrile (Note 4) present in the distillation flask can be recovered. The residue is broken up with 75 ml. of methanol, the mixture stirred and cooled, and the product recovered by filtration. Recrystallization from methanol gives 17-20 g. of crystalline material, m.p. 86-88°. The proton magnetic resonance spectrum (chloroform-d) shows complex multiplets at 5 7.20-8.00. 

The checkers obtained 12.8-13.0 g. (52-53%), m.p. 84-86°, in the first crop and 2.7-3.4 g. (11-14%), m.p. 52-62°, in the second crop. Recrystallization of the former from methanol gave 11.5 g. of crystals, m.p. 84-86°, suggesting that the first crop is a pure single isomer. A proton magnetic resonance spectrum in chloroform-d of the second crop shows two singlets at 8 1.62 and 1.64 for the terf-butyl groups. Thus this material is a mixture of syn and anti isomers. Both the first and second crops proved equally useful for tcrf-butoxycarbonylation of an amino acid. 

Figure 12. Proton magnetic resonance spectrum of CTC-HC1 in methanol-d,. ... 

The proton magnetic resonance spectrum of indapamide was obtained from an approximately 50 mg/mL solution using deuterated methanol as the solvent. The spectrum is shown in Figure 4 and spectral assignments are listed in Table II. Figure 4 also shows the structural lettering applied to indapamide to facilitate proton NMR spectral assignment. 

The proton magnetic resonance spectrum of dipotassium phthalocyanine dicyanoferrate(II) and of an analogous methyl-substituted derivative has been recorded at 60 mc/sec in methanolic potassium cyanide with tetramethylsilane as an internal calibrant 92). 

Fig. 6. Proton magnetic resonance spectrum of methyl groups of methanol in a Co(II)—thiocyanate—methanol solution at —90°C (the field increases from left to right). Peak a, Co(CHjOH)5 peak b, cis-Co(CH30H)sNCS peak c, trans-ColCHsOHls NCS. Peaks d, e and f, g are the respective first and second side bands of the bulk methyl and hydroxy resonances. (From Vriesenga [134], by courtesy of The American Chemical Society.)...

The complexes (l,5-cyclooctadiene)(2,4-pentanedionato)-palladium(II) and platinum(II) tetrafluoroborate are air-stable solids, soluble in polar organic solvents such as chloroform, methylene chloride, acetonitrile, acetone, or methanol but insoluble in nonpolar solvents such as alkanes, benzene, or ether. Their solutions in acetone have conductivities typical of 1 1 electrolytes. Their proton magnetic resonance spectra (in CDC13 solutions, internal tetramethylsilane reference at 60 MHz.) show peaks due to coordinated cyclooctadiene at 3.78 and 6.7-7.4r (Pd) and at 4.25 and 6.9-7.6r (Pt) and due to the chelated /3-diketone at 4.39 and 7.88r (Pd) and at 4.15 and 7.81r (Pt) with the expected area ratios. In the spectrum of the platinum compound coupling with the 95Pt isotope (33 %... 

C -(Dimethylpropylamine)carbaundecaborane(12) is a white crystalline solid, m.p. 191-192°. It is very soluble in acetone and tetrahydrofuran, slightly soluble in chloroform and methanol, and insoluble in benzene and water. The infrared spectrum (Nujol and hexachlorobutadiene mulls) contains major absorption bands at 2988(m), 2561(vs), 1481(m), 1472(m), 1414(m), 1130(m), 1035(m), and 934(m) cm. h The proton nuclear magnetic resonance spectrum (acetone-de solution) exhibits... 

Attempts to generate thiocamphor (5)-methylide (44) by the addition of diazomethane to thiocamphor and subsequent N2-elimination from the [3-1-21-cycloadduct 43 led to enethiol ether 45 via a 1,4-H shift (Scheme 5.17). The formation of an unstable intermediate 43 was proposed on the basis of the proton nuclear magnetic resonance ( H NMR) spectrum of the crude mixture. The postulated intermediate 44 could not be intercepted by dipolarophiles or methanol, and did not undergo electrocyclization to give the corresponding thirrane (41). 

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