Hydrazine acetate synthesis
- Product Name:Hydrazine acetate
- CAS Number:7335-65-1
- Molecular formula:C2H8N2O2
- Molecular Weight:92.1
64-19-7
7335-65-1
General procedure for the synthesis of hydrazine acetate from glacial acetic acid: 85% hydrazine hydrate (28.5 mL, 0.5 mol) was added to a 100 mL round-bottomed flask, placed in an ice bath with stirring, and glacial acetic acid (28.6 mL, 0.5 mol) was slowly added dropwise, controlling the reaction temperature between 0-10°C. The reaction was carried out at room temperature. After the dropwise addition, the reaction mixture was continued to be stirred at room temperature for 40 min. Subsequently, water was removed from the reaction system by distillation under reduced pressure. A solvent mixture of chloroform and ethanol (1:1, 20 mL, v/v) was added to the remaining liquid and stirred in an ice bath to promote crystallization, and then the mixture was transferred to a 4°C refrigerator for further crystallization. Finally, the solvent was removed by evaporation under reduced pressure to give a white solid product (41.6 g, 90.5% yield).
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Yield:7335-65-1 90.5%
Reaction Conditions:
with hydrazine hydrate at 0 - 20; for 0.666667 h;
Steps:
1 Hydrazine acetate (Intermediate 1)
in 100ml of round bottom flask add 85% of Hydrazine hydrate(28. 5ml, 0. 5mol), ice bath with stirring and was slowly added dropwise ice acetic acid(28.6ml0. 5mol) to control the temperature at 0-10 ° C. After the completion ofthe dropwise addition the reaction mixturewas stirred at room temperature for 40min. After distillation under reducedpressure to remove water, in the remaining liquid add Chloroform: ethanol (1:1,20ml), in the ice bath was stirred forcrystallization, and then placed in 4 ° C refrigerator for further crystallization then evaporated to dryness under reduced pressureto give a white solid (41. 6g, 90. 5%).
References:
Shanghai Institute of Pharmaceutical Industry;Shen, Shunyi;Yuan, Fang;Ge, Han;Zhang, Zhihong;Liu, Yubin CN102786570, 2016, B Location in patent:Paragraph 0074; 0075