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ChemicalBook CAS DataBase List Acethydrazide
1068-57-1

Acethydrazide synthesis

13synthesis methods
A kind of preparation method of acethydrazide include the following steps: Under nitrogen protection, by acetic acid, hydrazine hydrate It is put into catalyst in the reaction kettle with rectifying column, opens stirring, be heated to reflux, after steam enters rectifying column, Vapor are produced in tower top temperature for 98 DEG C~100 DEG C, when reaction 4~6 is small at a reflux temperature, when rectifying tower top frozen-free current Reaction terminates after going out, and continues heating distillation, and the acetic acid and hydrazine hydrate of reaction are had neither part nor lot in 100 DEG C~120 DEG C extraction of tower top temperature, After acetic acid and hydrazine hydrate are all steamed, liquid in kettle is poured out into filtering while hot, filtrate is through crystallisation by cooling, pure water, very Acethydrazide finished product is obtained after sky is dry.
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Yield:1068-57-1 98%

Reaction Conditions:

with hydrazine hydrate at 40 - 75; for 4 h;Green chemistry;Large scale;Temperature;

Steps:

1.1 Example 1 Preparation of pymetrozine.
(1) Preparation of hydrazide:1000 g of methyl acetate (solvent) was put into a 3000 ml three-necked flask,Under stirring conditions,500 g of hydrazine hydrate was slowly added dropwise to the three-necked flask, and the dropping time was controlled to 2 hours. The temperature of the reaction solution was controlled to 40 to 45C.After the dropwise addition, the temperature was raised to 75 ° C for 4 h. Cooled to room temperature,After solidification and crystallization (cooling to below 0 ° C) to give solid acetylHydrazine 725 g, yield: 98%.

References:

Jiangsu Anbang Electrochemistry Co., Ltd.;Ji Yuxiang;Jiang Yutian;Yao Xiuyu;Wang Junsheng;Long Xiguo;Zheng Chen;Xie Jun CN103724327, 2017, B Location in patent:Paragraph 0006; 0030; 0031; 0036; 0037; 0038; 0039

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