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Glufosinate ammonium preparation method

A technology of glufosinate-ammonium and methyl phosphonite is applied in the new preparation field of herbicide glufosinate-ammonium, which can solve the problems of expensive phthalimide, poor atom economy and low yield, etc. Atomic economy, easy operation, and easy availability of raw materials

Active Publication Date: 2018-06-15
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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AI Technical Summary

Problems solved by technology

[0013] Although the reaction conditions of this method are not high, the raw material phthalimide is more expensive, the atom economy is poor, and the yield is not high.

Method used

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Embodiment 1

[0029] Step 1: Add α-bromo-γ-butyrolactone 2 (16.5g, 0.1mmol) and sodium nitrite (13.8g, 0.2mmol) into a 100mL reaction flask filled with DMF (20mL), and stir at room temperature for 30min The response is complete. After the completion, 50 mL of ethyl acetate was added for dilution, and then washed with water (80 mL×3) to remove DMF, and the organic phase was concentrated to obtain 10.2 g of α-nitro-γ-butyrolactone 3, which was directly used in the next reaction, with a yield of 78%.

[0030] Step 2: Add compound 3 (39.3g, 0.3mmol), 45% hydrobromic acid (75mL), and methanol (150mL) to a 500mL reaction flask sequentially, heat up to 75°C and reflux for 4h, then cool down to room temperature, and stir overnight. After the reaction was completed, the solvent was removed under reduced pressure, and the obtained crude product was dissolved in ethyl acetate (150 mL), washed successively with saturated sodium bicarbonate solution and saturated brine (150 mL), dried over anhydrous mag...

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Abstract

The invention relates to a glufosinate ammonium preparation method. According to the present invention, nitro is introduced by using a simple and economical method, and is reduced under a mild condition so as to introduce amino group as the key step, such that the method for introducing amino by using other expensive amino acid derivatives or other toxic nitrogen-containing compounds is avoided, and the amino protection and deprotection during the reaction is eliminated; and the preparation method has advantages of simple reaction process, mild condition, simple and easily-available raw materials, simple operation and good atom economy, and is extremely suitable for industrial production.

Description

technical field [0001] The invention belongs to the fields of organic synthesis and pesticide synthesis, and specifically relates to a new preparation method of the herbicide glufosinate-ammonium. Background technique [0002] Glufosinate-ammonium is a highly efficient, low-toxic, non-selective (killing) contact organophosphorus herbicide with partial systemic effect. It was first developed and produced by the German Hoechst company in the 1980s. In addition to herbicidal activity, it also has insecticidal and fungicidal activity, and can be mixed with insecticides to achieve simultaneous control effects. The herbicide has high-efficiency herbicidal activity and can control almost all kinds of weeds. At the same time, it has the characteristics of low toxicity, easy degradation, water can be used as a base agent, and it is not easy to produce drug resistance, making it safe and convenient to use. At present, glufosinate-ammonium is used second only to glyphosate, and it is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 王继宇陈续玲张远康
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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