In a systematic investigation, the synthesis of metal–organic frameworks (MOFs) with MIL-140 structure was studied. The precursors of this family of MOFs are the same as for the formation of the well-known UiO-type MOFs although the synthesis temperature for MIL-140 is significantly higher. This study is focused on the formation of Zr-based MIL-140 MOFs with terephthalic acid (H2bdc), biphenyl-4,4′-dicarboxylic acid (H2bpdc), and 4,4′-stilbenedicarboxylic acid (H2sdc) and the introduction of synthesis field diagrams to discover parameters for phase-pure products. In this context, a MIL-140 network with H2sdc as linker molecule is first reported. Additionally, an important aspect is the reduction of the synthesis temperature to make MIL-140 MOFs more accessible even though linkers with a more delicate nature are used. The solvothermal syntheses were conducted in highly concentrated reaction mixtures whereby a targeted synthesis to yield the MIL-140 phase is possible. Furthermore, the effect of the often-used modulator approach is examined for these systems. Finally, the characteristics of the synthesized MOFs are compared with physisorption measurements, thermogravimetric analyses, and scanning electron microscopy.