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182 Chapter 7
D5
This sample was repeated following the reported method. [140] H3BTC (50mg, 0.24 mmol)
and 1 molar equivalent of ip (40mg, 0.24 mmol) combined with Cu(NO3)2·3H2O (171mg,
0.70 mmol) was placed into a 20ml screw jaw. Subsequently, 7 ml DMF and 0.3 ml conc.
HBF4 was added. The screw jaw was then sealed and put into a pre-heated oven at 80 °C
for 20 h. The resulting blue powder products were collected by centrifugation.
Afterwards, they were washed by DMF(30 ml x 3), EtOH (30 ml x 3) and acetone (30 ml x
3) subsequently. The final powder was collected and dried under air at room temperature.
The activation of the solids was performed by heating at 140 °C for 24 h under dynamic
vacuum (ca. 10 -3 mbar).
Figure 7.19. 1 H-NMR spectra of the acid-digest D5 sample (solvent: DMSO-d 6 , DCl).