Over the past 20 years, ⁶⁸Ga-labelled radiopharmaceuticals have become an important part in clinical routine. However, the worldwide supply with ⁶⁸Ge/⁶⁸Ga generators is limited as well as the number of patient doses per batch of ⁶⁸Ga radiopharmaceutical. In the recent years, a new technique appeared, making use of the ease of aqueous labelling via chelators as with ⁶⁸Ga but using ¹⁸F instead. This technique takes advantage of the strong coordinative bond between aluminium and fluoride, realized in the aqueous cation [Al¹⁸F]²⁺. Most applications to date make use of one-pot syntheses with free Al(III) ions in the system. In contrast, we investigated the labelling approach split into two steps: generating the Al-bearing precursor in pure form and using this Al compound as a precursor in the labelling step with aqueous [¹⁸F]fluoride. Hence, no free Al³⁺ ions are present in the labelling step. We investigated the impact of parameters: temperature, pH, addition of organic solvent, and reaction time using the model chelator NH₂-MPAA-NODA. With optimized parameters we could stably achieve a 80% radiochemical yield exerting a 30-min reaction time at 100 °C. This technique has the potential to become an important approach in radiopharmaceutical syntheses.