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Abstract The identification of silicon‐substituted, complex organics carrying multiple functional groups by classical infrared spectroscopy is challenging because the group frequencies of functional groups often overlap. Photoionization (PI) reflectron time‐of‐fight mass spectrometry (ReTOF‐MS) in combination with temperature‐programmed desorption (TPD) holds certain advantages because molecules are identified after sublimation from the matrix into in the gas phase based on distinct ionization energies and sublimation temperatures. In this study, we reveal the detection of 1‐silaglycolaldehyde (HSiOCH₂OH), 2‐sila‐acetic acid (H₃SiCOOH), and 1,2‐disila‐acetaldehyde (H₃SiSiHO)—the silicon analogues of the well‐known glycolaldehyde (HCOCH₂OH), acetic acid (H₃CCOOH), and acetaldehyde (H₃CCHO), in the gas phase after preparation in silane (SiH₄)–carbon dioxide ices exposed to energetic electrons and subliming the neutral reaction products formed within the ices into the gas phase.