In its fully optimized form, the reductive Kolbe heterocoupling of carboxylic acids takes place through a convenient one pot procedure, which does not require rigorous degassing and anhydrous conditions (Table ). The general procedure proceeds as follows: to a mixture of acid components (the less expensive of which is used in 3 equiv.) in CH 2 Cl 2 are added DIC and NHPI (1.1 equiv each relative to total acid quantity, 4.4 equiv total) along with catalytic amount of DMAP (10 mol% to total acid quantity, 0.4 equiv total). After stirring for 1 h, without any solvent removal, the solution is diluted with DMF and NiCl 2 •dme along with L4 are added (ca. 5 mol% each relative to total acid quantity, 20 mol% total), followed by the addition of NaI (0.2 M). Electrolysis using a standard ElectraSyn2.0 potentiostat (Zn anode and Ni foam cathode) for about 2.5 h (0.1 mmol scale) followed by standard workup and purification delivers the coupled product.