The CO stream is generated on‐site ex‐situ by thermal decomposition of Mo(CO)6 in the presence of DBU (dioxane, 65°C, 20 h; step 1) in a second, connected chamber.

Two different protocols are used for the synthesis of functionalized quinolones.

The formation of the title compounds is carried out in a two‐chambered system: first, an alkyl radical is generated which subsequently is subjected to aminocarbonylation, where CO is released from molybdenum hexacarbonyl.