Synthesis, characterization and molecular structure of [1-HOCPh2-2-NHMe2C6H4][MeSO3] · MeSO3H

BEt2(OSO2CH3) was treated with 1-HOCPh2-2-NMe2C6H4 (1) in the presence of acetic acid to give a red oily residue, which was separated by column chromatography into the two products [1-HOCPh2-2-NHMe2C6H4][MeSO3] · MeSO3H (2) and the known compound (BEt)2(μ-O)(μ-O,O′-O2CCH3)2 (3). Compound 2 was prepared independently from 1 and methylsulfonic acid. Compound 2 was characterized spectroscopically (NMR, IR) and by crystal structure determination. The latter shows the association of two ions and one molecule [1-HOCPh2-2-NHMe2C6H4]+, [MeSO3]− and MeSO3H by hydrogen bonding.

Graphical abstract[1-HOCPh2-2-NHMe2C6H4][MeSO3] · MeSO3H (2) was prepared from 1-HOCPh2-2-NMe2C6H4 and methylsulfonic acid and was characterized spectroscopically (NMR, IR) and by crystal structure determination. The latter shows the association of two ions [1-HOCPh2-2-NHMe2C6H4]+ and [MeSO3]− and one molecule MeSO3H by hydrogen bonding.Figure optionsDownload full-size imageDownload as PowerPoint slide