Method for synthesizing 3-nitro or 3-amino phthalyl hydrazine

A technology of nitrophthalic hydrazide and amino phthalic hydrazide is applied in the field of direct synthesis of 3-nitro phthalic hydrazide or 3-amino phthalic hydrazide, and can solve the problem of product Unstable quality, more waste water and other problems, to achieve the effect of simple operation, advanced and reasonable process

Inactive Publication Date: 2006-08-23
潘健
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method produces a lot of waste water, and the product quality is not stable

Method used

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  • Method for synthesizing 3-nitro or 3-amino phthalyl hydrazine
  • Method for synthesizing 3-nitro or 3-amino phthalyl hydrazine
  • Method for synthesizing 3-nitro or 3-amino phthalyl hydrazine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The synthesis of embodiment 1.3-nitrophthalohydrazide

[0015] In a dry 1000ml three-neck flask, add 100g of dimethyl 3-nitrophthalate, 140g of ethanol, and 83.6g of hydrazine hydrate (50%), stir and heat to reflux, maintain the reflux reaction for 3h, stir to lower the temperature, and cool to Suction filter after room temperature. The crystals were dissolved in water and filtered, and the solution was acidified with concentrated hydrochloric acid to pH 1.5-2, filtered, washed with water, and dried to obtain 60 g. The appearance was light yellow crystalline powder, the yield was 69%, the purity was 98.2%, and the melting point was >300°C. Infrared spectrogram see figure 1 .

Embodiment 2

[0016] The synthesis of embodiment 2.3-nitrophthalohydrazide

[0017] Add 100g of dimethyl 3-nitrophthalate, 200g of methanol, and 63g of hydrazine hydrate (40%) into a dry 1000ml three-neck flask, stir and heat to reflux, maintain reflux for 2 hours, stir to lower the temperature, and cool to room temperature After suction filtration. The crystals were dissolved in water and filtered, and the solution was acidified with concentrated hydrochloric acid to pH 1.5-2, filtered, washed with water, and dried to obtain 58g. The appearance was light yellow crystalline powder, the yield was 67%, the purity was 98.2%, and the melting point was >300°C. Infrared spectrogram see figure 1 .

Embodiment 3

[0018] The synthesis of embodiment 3.3-nitrophthalohydrazide

[0019] Add 100g of dimethyl 3-nitrophthalate, 80g of ethanol, and 171g of hydrazine hydrate (60%) into a dry 1000ml three-neck flask, stir and heat to reflux, maintain reflux for 4 hours, stir to lower the temperature, and cool to room temperature After suction filtration. The crystals were dissolved in water and filtered, and the solution was acidified with concentrated hydrochloric acid to pH 1.5-2, filtered, washed with water, and dried to obtain 62 g of 3-nitrophthalhydrazide, which appeared as a light yellow crystalline powder with a yield of 72%. The purity is 98.2%, the melting point is >300°C, and its infrared spectrum is shown in figure 1 .

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Abstract

The method of synthesizing 3-nitro phthalyl hydrazine or 3-amino phthalyl hydrazine is to react 3-nitro dimethyl phthalate and hydrazine hydrate in the weight ratio of 1 to 0.25-1.05 inside ethyl alcohol or methyl alcohol in the amount of 0.8-4 times the weight of 3-nitro dimethyl phthalate at 80-85 deg.c in the presence or absence of catalyst for 2-6 hr before cooling to crystallize and filtering to obtain crude 3-nitro phthalyl hydrazine or 3-amino phthalyl hydrazine product.

Description

technical field [0001] The invention relates to a method for directly synthesizing 3-nitrophthalhydrazide or 3-aminophthalhydrazide by using 3-nitrophthalate dimethyl as a starting material. Background technique [0002] The method for preparing 3-nitrophthalhydrazide is disclosed at present, which is obtained by high-temperature reaction of 3-nitrophthalic acid and hydrazine sulfate (refer to: editor-in-chief of Horning EC, translated by the teaching and research group of organic chemistry of Nanjing University, "Organic Synthesis" Episode 3, Beijing: Science Press 1981, 404). This method has high reaction temperature, serious pollution, cumbersome operation, and is not suitable for industrialized production. Secondly, the method for preparing 3-aminophthalhydrazide is formed by the reaction of 3-nitrophthalhydrazide and sodium dithionite (referring to: editor-in-chief of Horning EC, translated by the teaching and research group of organic chemistry of Nanjing University, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D237/32
Inventor 潘健
Owner 潘健
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