Preparation method of glufosinate intermediate

An intermediate, the technology of glufosinate-ammonium, which is applied in the field of preparation of glufosinate-ammonium intermediate 3-phosphonopropyl acetal diethyl alcohol, can solve the problems of low yield and poor atom economy, and achieve high yield and low cost , the effect of mild reaction conditions

Inactive Publication Date: 2019-01-18
NANJING REDSUN BIOCHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the invention is to provide a kind of glufosinate-ammonium intermediate 3-( A preparation method of methyl ethoxy) phosphono propionyl diethyl alcohol, the method is simple in process, low in cost, mild in reaction conditions, high in yield and good in atom economy

Method used

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  • Preparation method of glufosinate intermediate

Examples

Experimental program
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Effect test

Embodiment 1

[0022] 136g diethyl methyl phosphite, 460g dehydrated alcohol and 1.0g heterobimetallic molecular sieve type catalyst CuZr / ZSM-5 (3.5% of the loading capacity of Cu, 2.2% of the loading capacity of Zr) drop into the reaction vessel and mix, cool to 10°C; pass through nitrogen protection, slowly drop 56g of acrolein into the mixed solution, control the dropping temperature at 15-20°C, after the dropwise addition, control the temperature at 25-30°C, react for 4 hours, and depressurize after the reaction Concentrate by distillation and distill off ethanol to obtain 226 g of acetal with a normalized content of 97% and a yield of 92%.

Embodiment 2

[0024] 136g of diethyl methylphosphite, 460g of absolute ethanol and 2.5g of heterobimetallic molecular sieve catalyst CuZr / ZSM-5 (same as Example 1) were put into the reaction vessel and mixed, cooled to 10°C; Slowly add 58g of acrolein dropwise into the mixed solution, the dropping temperature is controlled at 15-20°C, after the dropwise addition is completed, the temperature is controlled at 25-30°C, and the reaction is carried out for 3 hours. The monochemical content is 98%, and the yield is 96%.

Embodiment 3

[0026] 136g diethyl methylphosphite, 460g absolute ethanol and 4.0g heterobimetallic molecular sieve catalyst CuZr / ZSM-5 (same as Example 1) were put into the reaction vessel and mixed, cooled to 10°C; Slowly add 58g of acrolein dropwise into the mixed solution, the dropping temperature is controlled at 15-20°C, after the dropwise addition is completed, the temperature is controlled at 25-30°C, and the reaction is carried out for 1 hour. The monochemical content is 97%, and the yield is 94%.

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Abstract

The invention discloses a preparation method of a glufosinate intermediate. Under the existence of heterobimetallic molecular sieve type catalyst CuZr / ZSM-5, acrylic aldehyde is dropwise added into amixed solution of methyl diethyl phosphite and absolute ethyl alcohol for reaction; after the reaction is completed, vacuum concentration is performed; the glufosinate intermediate of 3-(methyl ethyloxy) phosphonopropylal diethanol is obtained. The method has the advantages that the process is simple; the operation is easy; the reaction conditions are mild; the yield is high; the atom economy is high; the catalyst can be easily recovered and utilized; the industrial prospects are good.

Description

technical field [0001] The invention relates to a preparation method of a glufosinate-ammonium intermediate, in particular to a preparation method of the glufosinate-ammonium intermediate 3-(methylethoxy)phosphonopropionyl diethyl alcohol. Background technique [0002] 3-(Methylethoxy) phosphonopropyl acetal diethanol (structure shown in formula I) - acetal is an intermediate of the herbicide glufosinate-ammonium, especially through the Strecker route to synthesize glufosinate-ammonium An important intermediate of phosphine. [0003] [0004] Patent US6359162B1 uses diethyl methyl phosphite, acrolein, ethanol and acetic anhydride as raw materials to prepare acetal, the selectivity of the reaction is poor, the yield of acetal is not high, and acetic anhydride participates in the reaction, which increases the cost of raw materials, and Accompanied by the by-product formation of ethyl acetate, further treatment is required. Contents of the invention [0005] The object o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/32
CPCC07F9/3211C07F9/3264Y02P20/584
Inventor 李恒虎张兰平薛谊邢平王福军岳瑞宽
Owner NANJING REDSUN BIOCHEM CO LTD
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