resolver

180 Chapter 7
D3
The mixture of H3BTC (100mg, 0.48 mmol), ip (80 mg, 0.48 mmol) and Cu(BF4)2 6H2O
(488 mg, 1.4 mmol) was placed into a 50 ml Teflon vessel. Subsequently, 24 ml EtOH was
added. The Teflon reaction vessel was then placed in the Teflon-lined stainless steel
autoclaves. The autoclaves were further sealed and placed into the pre-heated oven at 80
°C for 20 h. Afterwards the autoclaves were taken out and cooled down at room
temperature. The resulting blue powder products were separated from the solution by
centrifugation. Afterwards, they were washed by EtOH (30 ml x 3) and acetone (30 ml x
3) subsequently. Finally, the solvent was removed and the powder was dried under
ambient atmosphere at room temperature. The activation of the solids was performed by
heating at 120 °C for 24 h under dynamic vacuum (ca. 10 -3 mbar).
Figure 7.17. 1 H-NMR spectra of the acid-digest D3 sample (solvent: DMSO-d 6 , DCl).