2,2-Dimethyl-1,3-dioxolane-4-carboxylic acid-13C3 is an intermediate for the synthesis of 2,3-DPG-13C3 Sodium Salt (D491993), which is a labeled isotope of 2,3-Diphospho-D-glyceric Acid, a metabolite formed in the metabolomes of normal and sickle cell erythrocytes.
2,2-Dimethyl-1,3-dioxolane-4-methanol (350 mg, 1.1 mmol) was used as a raw material and mixed with RuCl3 (318 mg, 1.1 mmol) in a solvent mixture of acetonitrile (10 mL) and water (5 mL). K2CO3 (455 mg, 3.3 mmol), trichloroisocyanuric acid (TCCA) and tetrabutylammonium bromide (TBAB) were subsequently added. The reaction mixture was stirred at room temperature for 3 hours. Upon completion of the reaction, the reaction was quenched with aqueous ammonium chloride and extracted with ethyl acetate. The organic layers were combined, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to afford 2,2-dimethyl-1,3-dioxolane-4-carboxylic acid (450 mg, 75% yield). LC-MS analysis showed m/z = 147.4 [M + H]+.
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