It is a significant challenge to construct chiral metal−organic frameworks (CMOFs) by developing a facile and green preparation strategy. In this work, CMOFs were first synthesized via a mechanochemical process by combining a truncated mixed ligand strategy and defect engineering theory. The simple, green, and rapid construction strategy could solventfreely harvest gram-scale CMOFs with a hierarchical micro/ mesoporous structure. The as-synthesized CMOFs were evaluated by Aldol asymmetric catalysis and exhibited excellent catalytic performance (conversion was up to 97.1%, the ee value was 44.3%, and the activity was still good after 5 cycles).

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Green, facile, and large-scale preparation of functionalized metal−organic frameworks (MOFs) remains a challenge. Herein, we report a rapid synthesis of functionalized MOFs by the integration of post-synthetic ligand exchange (PSLE) and mechanochemistry. This mechano-PSLE approach can circumvent the hurdles of PSLE such as long reaction time, excessive solvent, and even failure of PSLE caused by redissolution and recrystallization under solvothermal conditions. More importantly, the gramscale MOF functionalized with the chiral group can be obtained facilely and greenly. It exhibited excellent asymmetric catalytic performance (81% conversion and 92.1% ee) for α-alkylation of aldehydes irradiated by a xenon lamp, providing a basis for industrial batch production of functionalized MOFs.