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Under hydrothermal (solvothermal) reaction conditions chiral compounds 1, 2, and 3and one acentric compound 4were obtained by the reaction of Zn2+or Cd2+with racemic 3‐(3‐pyridyl)‐3‐aminopropionic acid (rac‐HPAPA). Compounds 1and 2crystallized in chiral space group P212121. At 105 °C, racemic 3‐pyridyl‐3‐aminopropionic acid (rac‐HPAPA) reacted with Zn(ClO4)2⋅6 H2O and dehydrogenated in situ to form the first chiral coordination polymer [Zn{(E)‐3‐C5H4NC(NH2)CHCOO}]ClO4(1) with a β‐dehydroamino acid. Beyond 120 °C, the reaction of rac‐HPAPA with Zn(ClO4)2⋅6 H2O deaminates in situ to form chiral coordination polymer [Zn{(E)‐3‐C5H4NCHCHCOO}(OH)] (2). At relatively low temperatures (70 °C), the solvothermal reaction of Zn(NO3)2⋅6 H2O with rac‐HPAPA in methanol does not lead to any change in the ligand and results in the formation of a chiral (P212121) coordination polymer [Zn(papa)(NO3)] (3). The same reaction of Cd(ClO4)2⋅6 H2O with HPAPA also does not lead to any change in ligand and results in the formation of noncentric (Cc) coordination polymer [Cd(papa)(Hpapa)]ClO4⋅H2O (4). The network topology of both 1and 3is 10,3a, while 2has a diamondoid‐like (KDP‐like, KDP=potassium dideuterophosphate) network. Particularly interesting from a topological perspective is that 4has an unprecedented three‐dimensional network. Compounds 1, 2, 3, and 4are all second harmonic generation (SHG) active with 1exhibiting the strongest response, while only 4also displays good ferroelectric properties.