2206-26-0

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• Synthesis

  In a glove box, the tridentate complex of manganese catalyst (0.005 mmol, 1 mol%) was added to a 100 mL Schlenk tube equipped with a stir bar. Acetonitrile (0.5 mmol, 1.0 equivalent) was then added to the reaction tube using a glass pipette, followed by degassed toluene (0.5 mL) using the same pipette. The solution was stirred at room temperature for 10 minutes, and then degassed D₂O (0.5 mL) was added. The Schlenk tube was removed from the glove box, and the reaction mixture was stirred at 110°C (oil bath) for 24 hours. After the reaction was complete, ethyl acetate was added to the reaction system, and the reaction mixture was extracted with ethyl acetate. The organic layer was separated, and the ethyl acetate solution was dried over anhydrous sodium sulfate. The anhydrous sodium sulfate solid was removed by filtration. The filtrate was then purified by vacuum to remove the solvent (it should be noted that deuterated acetonitrile has a low boiling point, and special attention should be paid to the vacuum level and evaporation temperature during vacuum concentration) to obtain the target product molecule, deuterated acetonitrile.
  

  

  Figure: Synthetic Route of ACETONITRILE-D3

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