Nuclear magnetic resonance spectra methanol

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... 

Illustration of hydrolysis A represents the methoxysilane signal and B the methanol resonance in an extract of a nuclear magnetic resonance spectrum. The decrease of A versus the increase of B indicates that hydrolysis is taking place. Once the intensity of B is constant the reaction is complete... 

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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