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Synthetic method of methyl phosphite and glufosinate-ammonium

A technology of methyl phosphonite and synthesis method, which is applied in the synthesis field of organophosphorus compounds, can solve the problems of high requirements, potential safety hazards, personal injury of operators, etc., and achieves improvement of synthesis yield, reduction of emissions, and reduction of environmental protection. Effects of cost and pressure

Inactive Publication Date: 2016-04-27
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This synthesis method has high requirements in the actual operation process, and is not suitable for the simple operation of the factory, which accordingly restricts the company's large-scale production; at the same time, there are potential safety hazards that cause personal injury to the operators.

Method used

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  • Synthetic method of methyl phosphite and glufosinate-ammonium
  • Synthetic method of methyl phosphite and glufosinate-ammonium
  • Synthetic method of methyl phosphite and glufosinate-ammonium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 111.1gP in a 500ml four-neck flask 2 S 5 (0.25mol) and 1.2gDMAP (0.01mol), add 46g ethanol (1mol) in the constant pressure titration funnel, when the temperature rises to 70 ℃, start to drop ethanol, and control the reaction temperature at 60-100 ℃, when the specific gravity of the material liquid reaches At 1.170-1.180, the dropwise addition is completed, keep warm for 20-30min, and start to cool down to obtain the crude sulfide (I).

[0030] When the temperature of the sulfide crude product (I) dropped to 35°C, pass 71g of chlorine gas (1mol) to carry out the chlorination reaction, control the flow of chlorine gas, absorb the tail gas with 1000g of deionized water, measure the specific gravity of the material and liquid every 2 hours, and control the chlorination The temperature is between 35-50°C, and the reaction is stopped when the specific gravity of the reaction solution is 1.275-1.285, and the crude chloride (II) is obtained.

[0031] Add dropwise 19.5gNa ...

Embodiment 2

[0035] The method is the same as in Example 1, and the specific parameters are shown in Table 1, Table 2, and Table 3. The distilled refined chlorophosphonite is directly used as a hydrogenation raw material in a fixed-bed reactor for catalytic reaction. Use a tubular reactor with an inner diameter of 32mm, load 20g of metal catalyst (20-40 mesh), the active components are Ni, Cu, Pt, the additives are Zr, Ce, and the carrier is γ-Al 2 o 3 .

Embodiment 3

[0037] The method is the same as in Example 1, and the specific parameters are shown in Table 1, Table 2, and Table 3. The distilled refined chlorophosphonite is directly used as a hydrogenation raw material in a fixed-bed reactor for catalytic reaction. A tubular reactor with an inner diameter of 32 mm was used to load 20 g of metal catalyst (20-40 mesh), the active components of which were Rh and Pt, the auxiliary agents were Y and La, and the carrier was 5A molecular sieve.

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Abstract

The invention discloses a synthetic method of methyl phosphite and glufosinate-ammonium. The method comprises the steps: with phosphorus pentasulfide as a starting material, then carrying out vulcanization reaction, chlorination reaction, water washing and distillation purification, then carrying out catalytic hydrogenation to obtain chloride phosphite (III), and next carrying out Grignard reaction to obtain methyl phosphite (IV), wherein R is C1-C4 alkyl. The method comprises the steps: with phosphorus pentasulfide as the starting material, then carrying out vulcanization reaction, chlorination reaction, water washing and distillation purification, then carrying out catalytic hydrogenation to obtain chloride phosphite, next carrying out Grignard reaction to synthesize methyl phosphite (IV), and thus obtaining the final product glufosinate-ammonium through a Strecker route of the prior art. The synthetic yield is increased, methyl phosphorus dichloride and other unstable corrosive intermediates cannot be produced, the discharge of three-waste substances is reduced, and environment-friendly costs and pressure are reduced.

Description

technical field [0001] The invention relates to a synthesis method of an organophosphorus compound, in particular to a synthesis method of methyl phosphonite and glufosinate-ammonium. Background technique [0002] Glufosinate-ammonium (glufosinate~ammonium) was developed and produced by Hoechest in the 1980s. Its chemical name is 4~[hydroxy (methyl)phosphono]~DL~homoalanine, also known as glufosinate-ammonium ammonium salt. Phosphonic acid herbicides are glutamine synthesis inhibitors, non-selective (killing) contact herbicides. The most important intermediate product in the current glufosinate-ammonium synthesis mainstream route is methyl phosphonite (IV), wherein R on the methyl phosphonite is C 1 ~C 4 The alkyl group, methyl phosphonite obtains final product glufosinate-ammonium through the strecker route of prior art, therefore, the preparation of intermediate is the key step of synthetic glufosinate-ammonium. [0003] The preparation of diethyl methylphosphonite is i...

Claims

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Application Information

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IPC IPC(8): C07F9/48C07F9/30
CPCC07F9/4816C07F9/301
Inventor 刘善和黄永升方红新葛德强吴李瑞仲崇凤王红伟杨继华
Owner ANHUI COSTAR BIOCHEM CO LTD
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