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Efficient and environmentally-friendly method for preparing 6-chloro-2-quinoxaline phenol

A quinoxaline phenol, an environmentally friendly technology, applied in the field of synthesis of the important intermediate 6-chloro-2-quinoxaline phenol, can solve the problems of high catalyst price, large pollution, poor selectivity, etc.

Inactive Publication Date: 2012-07-18
JIANGSU FENGSHAN GROUP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In summary, although the chemical reduction method has a high yield, it is highly polluting and prone to carcinogenic by-products
The method of catalytic reduction, the catalyst is expensive and the selectivity is not good

Method used

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  • Efficient and environmentally-friendly method for preparing 6-chloro-2-quinoxaline phenol

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Embodiment Construction

[0017] Below by embodiment the present invention is given further description, certainly the present invention is not limited to following embodiment

[0018] The preparation of catalyst, 50 kilograms of ferric trichloride hexahydrate is dissolved in the water of 2000 liters, adds 200 kilograms of active carbons, drips liquid caustic so that the pH value of solution is between 10-12, filters, dries to obtain 20% Fe(OH) 3 / C. In the 5000L reactor, drop into 2300 kilograms of metered 16% sodium hydroxide solution, drop into 425 kilograms of p-chloro-o-nitroacetoacetanilide in 5 times at 25°C, and react at this temperature for 1 hour, then Raise the temperature to 75°C-80°C within 1 hour, and keep it at this temperature for 1.5 hours, and throw 14 kg of 20% Fe(OH) 3 / C catalyst, add 100 kg of 80% hydrazine hydrate dropwise within 2 hours, the dropping temperature is 70°C-80°C, after the dropwise addition, the temperature is raised to 90°C, kept for 1 hour, then heated to 95°C, ...

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Abstract

The invention discloses an efficient and environmentally-friendly method for preparing 6-chloro-2-quinoxaline phenol. The method is characterized by comprising the following steps of: (1) dissolving p-chloro-o-nitroacetoanilide into a sodium hydrate or potassium hydrate solution, and reacting at the temperature of 70-90 DEG C for 2-8 hours; (2) adding an appropriate amount of catalyst, wherein the catalyst is ferric hydrate, FeOH / C or Fe(OH)3 / C; and (3) dropwise adding a hydrazine hydrate serving as a reducing agent, controlling the dripping temperature at 70-90 DEG C, preserving heat for 8 hours, cooling after reacting, filtering, and drying to obtain 6-chloro-2-quinoxaline phenol serving as a finished product. The method is characterized in that: a cheap and safe iron / active carbon catalyst is used, the hydrazine hydrate is taken as the reducing agent, nitrogen gas which is harmless to the environment is discharged in a reaction, an entire reaction system is efficient and environmentally-friendly and has low cost, and the method is convenient for industrial popularization.

Description

technical field [0001] The invention relates to the field of compound synthesis, in particular to the synthesis of an important intermediate 6-chloro-2-quinoxaline phenol of the pesticide herbicide quizalofop-p-ethyl. Background technique [0002] Quizalofop-ethyl is a post-emergence selective herbicide developed by Nissan Chemical Industry Co., Ltd., Japan. It is a systemic conduction-type selective stem and leaf treatment agent. The leaf crops are safe and can be widely used in the control of gramineous weeds in crops such as cotton, rapeseed, peanuts, soybeans and various broad-leaved vegetables. Quizalofop-p-ethyl has high safety, good rain resistance, prevents regeneration, does not reduce the effect at low temperature, is convenient to use, and has a special effect on completely destroying grass weeds, so its application and development prospects in the treatment of grass weed stems and leaves are very promising. broad. 6-Chloro-2-quinoxaline phenol is a very critica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/44
Inventor 谭波殷凤山王洪雷单永祥王波沈永强
Owner JIANGSU FENGSHAN GROUP
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