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• Synthesis

  4-Methyl-1-(3-methyl-2-pyridinyl)-2-phenylpiperazine, also known as mirtazapine impurity E, is a byproduct of mirtazapine production. The reaction process is as follows:
  
  i. CH3SO2Cl, CH2Cl2, reflux; ii. LiAlH4, THF, The specific reaction steps are as follows: Under a N2 atmosphere at 0-5°C, methanesulfonyl chloride (4.86 g, 42.45 mmol) was added to a solution of mirtazaol (10.0 g, 35.34 mmol) and triethylamine (5.35 g, 52.97 mmol) in dichloromethane (60 mL), and stirred at 25-30°C for 12 hours. Afterward, the mixture was heated under reflux for 2 hours. The mixture was cooled to 25-30°C, washed with water (20 mL), and the solvent was evaporated to obtain a methanesulfonyl derivative intermediate (10.22 g, 80%). The residue was dissolved in THF (100 mL) without purification, and LiAlH₄ (5.37 g, 141.32 mmol) was added under a N2 atmosphere at 0-5°C. The reactants were heated under reflux for 15 hours, quenched at 0°C with water (5.4 mL), 15% NaOH (5.4 mL), and water (16.2 mL), filtered, and the filtrate was evaporated to dryness and then added with diisopropyl ether (40 mL). The filtered product was washed with diisopropyl ether (10 mL) and dried to give mirtazapine impurity E (5.66 g, 75%) as a white solid with a purity of 99.1%.;

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