Fast and energy‐efficient synthesis methods become increasingly important aspects in the experimental high throughput searching of functional materials. Particularly high‐temperature solid‐state preparation techniques typically require large amounts of energy due to extended heating cycles. Therefore, we have utilized a time and energy‐efficient synthesis method using a commercial microwave oven in order to prepare intermetallic Laves‐type phases. Ti2M3Si with M = Mn, Fe, Co, Ni can be prepared within only 10 min of microwave heating based on this convenient one‐step procedure. These compounds are of interest because of their potentially useful magnetic properties and therefore contribute to the ongoing search for rare earth‐free alternatives to state‐of‐the‐art magnetic materials.Transition metal‐based Laves phase compounds Ti2M3Si were prepared by time‐ and energy‐efficient microwave heating and their structural and magnetic properties studied.