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Three aluminum compounds, namely alumina, aluminum hydroxide, and boehmite, are probed as the metal sources for the hydrothermal synthesis of a typical metal-organic framework MIL-53(Al). The process exhibits enhanced synthetic efficiency without the generation of strongly acidic byproducts. The time-course monitoring of conversion from different aluminum sources into MIL-53(Al) is achieved by multiple characterization that reveals a similar but differentiated crystallinity, porosity, and morphology relative to typical MIL-53(Al) prepared from water-soluble aluminum salts. Moreover, the prepared MIL-53(Al) constructed with the three insoluble aluminum sources exhibit an improved thermal stability of up to nearly 600 degrees C and enhanced yields. Alumina and boehmite are more preferable than aluminum hydroxide in terms of product porosity, yield, and reaction time. The adsorption performances of a typical environmental endocrine disruptor, dimethyl phthalate, on the prepared MIL-53(Al) samples are also investigated. The improved structural stability of MIL-53(Al) prepared from these alternative aluminum sources enables double-enhanced adsorption performance (up to 206 mg g(-1)) relative to the conventionally obtained MIL-53(Al).