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ACER FUNDED PROJECTS The basis and starting point for the mechanistic and experimental work was the hypothetical catalysis cycle with nickel alactones as intermediates (see Fig 42). On the basis of this, systems were investigated with which the oxidative coupling of ethylene and CO2 (A), the base-induced lactone cleavage (B) and the final ligand exchange (D) can be carried out.[2] The focus was on nickel-phosphane complexes, with the help of which suitable reaction con- ditions and bases should be identified in order to enable catalytic reaction control. Since NaOH reacts irreversibly with CO2 to form carbonates, which are not basic enough to in- itiate lactone cleavage, the choice of base was decisive in addition to the design of a suitable catalyst. The base should not react irrevers- ibly with CO2, enable lac- tone cleavage and can also be regenerated with NaOH. The extensive quantum mechanical calculations made it possible to ration- alise the experimental pro- cedure and specifically im- prove the system. [3b,4] Since no heterogeneous catalysts were known for this target reaction at the start of the project, more than 460 catalysts were investigated in nine differ- ent libraries using high-throughput experiments. In addition to the search for pure heterogeneous catalysts, hte also evaluated the extent to which de- fined nickel complexes or base can be heterogenized in order to simplify product separation or catalyst recycling. 1.13.3 Results First of all, a one-pot system was developed in which sodium acrylate could be produced catalytically with respect to the nickel used by repeating differ- ent reaction cycles (low CO2 atmosphere with addition of base; NaOMe as base). However, the highest turnovers here were only 10. Based on this system and the experiences with it, the first true style catalysis was achieved using Ni (COD) 2 in combination with a chelate phosphane ligand and fluorophenolate bases. [6,7] Fig. 42: Catalysis cycle of the nickel- catalysed NaAcrylate synthesis 103PDF Image | Chemical Processes and Use of CO2
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