The procedure for the desolvation of DUT-76(Cu) showed to be critical for the materials stability and physisorption behaviour. Specifically, a fast gas release for flushing as well as a release of the excess CO2 from the autoclave and a fast heating to generate supercritical CO2 have shown to lead to a degradation of the material. For this reason, we want to give detailed information on desolvation and thermal activation. Supercritical drying of the MOF powder after synthesis was performed in a Jumbo Critical Point Dryer 13200J AB (SPI Supplies). The MOF suspended in dry acetone was therefore transferred into the glass filters of the dryer. The autoclave was then filled with liquid CO2 at 290 K and 7.5 MPa. By opening the valve at the bottom of the autoclave the remaining acetone was removed while fresh liquid CO2 was refilled from the top of the autoclave. This procedure was repeated 8 times per day over two days until no acetone traces were observed in the dry ice at the outlet. In the following step, the valve from the gas cylinder into the dryer was closed and half the liquid CO2 in the autoclave was released. Then all valves of the autoclave were closed, and the temperature increased to 313 K to convert the CO2 into supercritical state. The pressure in the autoclave was maintained at 9 MPa during heat up. After equilibration of the system at 313 K overnight, the supercritical CO2 was released through the bottom valve over 12 hours.