The general procedure for the synthesis of methanesulfonyl hydrazine from methanesulfonyl chloride is as follows: 0.12 mol of ethanol solution of methanesulfonyl chloride was slowly added dropwise to an ethanol solution containing 0.62 mol of hydrazine hydrate, and the temperature of the reaction was maintained at 10-12 °C. After the dropwise addition, the reaction mixture was stirred at room temperature for 1 hour. After completion of the reaction, the solvent was removed by distillation under reduced pressure. Subsequently, the viscous residue was transferred to the ether phase over a period of 5 days using sequential extraction. Next, the ether was removed using a rotary evaporator. The final product was recrystallized by methyl acetate and allowed to stand at low temperature for several weeks until crystals precipitated.
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