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Preparation technology and content measuring method of triazole derivative preparation

A technology of preparation process and determination method, which is applied in the field of preparation process of triazole derivative preparations and its content determination, can solve problems such as increasing costs, and achieve the effects of reducing solvent use costs and high reaction speed

Inactive Publication Date: 2017-07-14
CHENGDU GREEN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if this method is applied in industry, it will greatly increase the cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 0.1 mol of o-nitrochlorobenzene, 0.4 mol of hydrazine hydrate, and 3 mmol of phase transfer catalyst into a three-necked flask, heat with magnetic stirring, and reflux for 5 hours. The reaction temperature is 110°C, and the stirring speed is 500 r / min. Add 40% sodium hydroxide solution to the solution, then use a rotary evaporator to evaporate and recover excess hydrazine hydrate, adjust the pH value of the solution to 3.0-3.5, filter with suction and wash with 10% ice-salt water, and vacuum dry to obtain triazole Derivatives, the yield is 99.3%.

[0018] Wherein, the phase-transfer catalyst that adopts in the present embodiment is PEG-800, with quaternary ammonium salt CTMAB, TBAB is that phase-transfer catalyst compares with polyethylene glycol (PEG) phase-transfer catalyst, and wherein quaternary ammonium salt phase catalyst is easy to decompose, In the liquid chromatography analysis chart, it can be seen that many by-products are generated. It can be seen from t...

Embodiment 2

[0028] Content detection of the triazole derivatives prepared in Example 1 was carried out by high performance liquid chromatography, chromatographic conditions: C18 (5um, diameter 4.6mmx150mm), UV detector, detection wavelength 254nm, column temperature 30°C , mobile phase: methanol aqueous solution 75:25 (v / v), flow rate is 1.0ml / min, sample size is 5ul, with standard solution concentration as X-axis, with peak area as Y-axis as standard curve, the measured The peak area of ​​benzotriazole was compared with the standard curve to obtain the content of the triazole derivative preparation.

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Abstract

The invention discloses a preparation technology and a content measuring method of a triazole derivative preparation. The preparation technology comprises the following steps: adding o-nitrochlorobenzene, hydrazine hydrate, and a phase transfer catalyst into a three-mouth flask, heating the mixture under magnetic stirring, stopping heating, adding a sodium hydroxide solution (40%) into the reaction liquid, evaporating excess hydrazine hydrate by a rotary evaporator, recovering evaporated hydrazine hydrate, adjusting the pH of the solution to 3.0-3.5, carrying out suction filtration, washing the filtrate by ice brine (10%), and drying the filtrate to obtain triazole derivatives. A phase transfer catalysis technology is used, namely, a phase transfer catalyst is added into a solution, a reactant is transferred into a phase containing another reactant, the whole reactions have a high reaction speed, the solvent cost is reduced, and the preparation technology is widely used in industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation process of a triazole derivative preparation and a content determination method thereof. Background technique [0002] The preparation process of triazole derivative preparations, such as the synthesis process of 1-hydroxybenzotriazole, mainly adopts the solvent method, that is, a certain solvent is added to the reaction solution to make the reaction proceed in a homogeneous phase. However, if this method is applied in industry, the cost will be greatly increased. [0003] Based on this, research and development of a preparation process of triazole derivative preparations. Contents of the invention [0004] The present invention now provides a preparation process for a triazole derivative preparation and a method for determining its content. By using phase transfer catalysis technology and adding a phase transfer catalyst, one reactant can be transferr...

Claims

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Application Information

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IPC IPC(8): C07D249/18G01N30/02
CPCC07D249/18G01N30/02
Inventor 周彩娥黄松董强梁正全程迪
Owner CHENGDU GREEN TECH CO LTD