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The MS/MS spectrum of the metastable molecular ions of dimethyl terephthalate 1 features an unexpected, quite intense, loss of a methyl radical. Using a combination of mass spectrometry techniques, it is shown that this process consists of a pseudo simple cleavage reaction isomerizing, in the first step, one of the two methoxycarbonyl substituents into a distonic ArC + (–OH)–OCH 2 ...
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