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A kind of 3-(alkoxymethylphosphoryl) propionate synthetic method

A technique for the synthesis of alkoxymethylphosphoryl groups, which is applied in the fields of fine chemicals and pesticides, can solve the problems of poor selectivity of acid-binding agents and temperature control, and achieve environmental friendliness, precise temperature control, and broad-scale application prospects Effect

Active Publication Date: 2018-09-28
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a new method for synthesizing propionate by the esterification reaction of bisacyl chlorides using a novel array tubular reaction device. And the problem of temperature control during the esterification reaction

Method used

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  • A kind of 3-(alkoxymethylphosphoryl) propionate synthetic method
  • A kind of 3-(alkoxymethylphosphoryl) propionate synthetic method
  • A kind of 3-(alkoxymethylphosphoryl) propionate synthetic method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-5

[0020] Weigh 37.8g of bisacyl chloride and 34g of methylene chloride and seal them in bottle A for later use, and weigh 36.8g of ethanol in bottle B. After the cooling circulation system was turned on to control different esterification temperatures, the bisacyl chloride solution and ethanol were pumped into the new array tube reaction device in proportion to carry out the esterification reaction by using micro-injection pumps respectively. The reaction solution is quenched with an acid-binding agent to collect the product, and the incoming and outgoing product is weighed. After the product was evaporated to dryness, it was washed and filtered with ethyl acetate, the solid was weighed, and the filtrate was weighed by rotary evaporation to dryness, and the sample was analyzed by GC and the yield was calculated. The data are shown in the table below:

[0021]

[0022] a Esterification conditions: n (双酰氯) :n (乙醇) =1:4; Bisacyl chloride solution feed rate: 5g / min.

Embodiment 6-11

[0024] Weigh 37.8 g of bisacyl chloride and 34 g of dichloromethane and seal them in bottle A for later use, and weigh ethanol in bottle B in different molar ratios. After turning on the cooling circulation system to the required temperature, the bisacyl chloride solution and ethanol were pumped into the new array tubular reaction device in proportion to carry out the esterification reaction by using a micro-injection pump respectively. The reaction solution is quenched with an acid-binding agent to collect the product, and the incoming and outgoing product is weighed. After the product was evaporated to dryness, it was washed and filtered with ethyl acetate, the solid was weighed, and the filtrate was weighed by rotary evaporation to dryness, and the sample was analyzed by GC and the yield was calculated. The data are shown in the table below:

[0025]

[0026]

[0027] b Esterification conditions: esterification temperature: -10°C; feeding rate of bisacyl chloride sol...

Embodiment 12-16

[0029] Weigh 37.8g of bisacyl chloride and 34g of methylene chloride and seal them in bottle A for later use, and weigh 36.8g of ethanol in bottle B. After turning on the cooling circulation system to the required temperature, the bisacyl chloride solution and ethanol were pumped into the new array tubular reaction device in proportion to carry out the esterification reaction using a micro-injection pump, and the feeding speed of different bisacyl chloride solutions was controlled. The reaction solution is quenched with an acid-binding agent to collect the product, and the incoming and outgoing product is weighed. After the product was evaporated to dryness, it was washed and filtered with ethyl acetate, the solid was weighed, and the filtrate was weighed by rotary evaporation to dryness, and the sample was analyzed by GC and the yield was calculated. The data are shown in the table below:

[0030]

[0031] c Esterification conditions: n (双酰氯) :n (乙醇) =1:4; Esterificatio...

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Abstract

The invention discloses a novel synthesis method for 3-(alkoxy methyl phosphoryl)propionate (short for "propionate") by carrying out esterification reaction on 3-(methyl phosphoryl chloride)propionyl chloride (short for "bis(acyl chloride) ") serving as a raw material. The method in which a novel array tubular reaction device is mainly adopted comprises the steps: feeding raw materials including bis(acyl chloride) and a hydroxyl compound from one side, then, releasing heat by reaction in glass tubes, enabling a condensed fluid to be in cross flow contact with the glass tube on the outer layer of a reaction tube, carrying out strong heat exchange, carrying out quenching treatment by using an acid binding agent after discharging as an esterification product, and then, collecting a product, so that continuous esterification synthesis reaction and sufficient heat exchange with a reaction solution can be realized, and an HCl gas serving as a byproduct has no corrosion to equipment. The method is simple in operation, high in heat exchange capability, precise in temperature control, environment-friendly and wide in large-scale application prospect.

Description

Technical field: [0001] The invention belongs to the fields of fine chemicals and pesticides, and in particular relates to a method for synthesizing glufosinate-ammonium intermediate propionate by adopting a novel array tubular reaction device to carry out esterification reaction of bisacyl chloride. Background technique: [0002] 3-(Alkoxymethylphosphoryl) propionate (referred to as "propionate") is an important synthetic intermediate of glufosinate-ammonium. It can be hydrolyzed directly after cyanamide to obtain glufosinate-ammonium. Glufosinate-ammonium is a new type of herbicide developed in the 1980s. At present, it is the second largest herbicide after glyphosate. Therefore, the array tubular reaction device has very important social significance and industrial application prospects not only for the synthesis of glufosinate-ammonium intermediates, but also for the development of many continuous high exothermic reactions. [0003] At present, the esterification react...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/32B01J19/00
CPCB01J19/0013C07F9/3211
Inventor 谷顺明黄永升周爱民张令伟张财华张志宏
Owner ANHUI COSTAR BIOCHEM CO LTD
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