Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of preparation method of saflufenacil

A technology of saflufenacil and sulfonyl diamide, which is applied in the field of preparation of saflufenacil, can solve the problems of many impurities in side reactions, difficult separation of condensing agents, high production costs, etc., and achieve high total yield, The effect of reducing industrial salt solid waste and three wastes

Active Publication Date: 2022-03-08
江苏乾元生物科技有限公司
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are mainly two kinds of synthetic methods reported in the literature: one is the condensation of acid intermediates and sulfonamides under the conditions of condensing agents, resulting in more three wastes and many impurities in side reactions, especially the by-products of condensing agents are difficult to separate and reuse The second is to use acid chloride intermediates and sulfonamides to condense under the condition of acid-binding agents. In the process, the same process involves the recovery of acid-binding agents or easily produces a large amount of high-concentration wastewater containing industrial salts, and the production cost is high.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of preparation method of saflufenacil
  • A kind of preparation method of saflufenacil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (Embodiment 1) Saflufenacil

[0021] Preparation of the target product in a small test:

[0022] Put 60.5g (0.20mol) of I-methyl intermediate and 100g of benzene into a 500mL glass bottle, heat and stir at 60°C, control the amount of chlorine gas 60g through the mass flow meter, and control the amount of I-methyl intermediate in the total material during the heat preservation The normalized content of liquid chromatography is less than 1%, the solvent is recovered by precipitation and the by-product hydrochloric acid is recovered by negative pressure to obtain the crude product of I-trichlorobenzyl intermediate, the by-product hydrochloric acid is recovered by solvent washing and liquid separation, and the recovery rate of solvent dehydration is 90%. Produce 28% hydrochloric acid 100g.

[0023] Under the protection of nitrogen, 150 g of dichloroethane and 30.5 g of sulfonamide intermediate were successively added to the above-mentioned 500 mL reaction vessel, stirred e...

Embodiment 2

[0025] Preparation of target product in pilot scale:

[0026] Put 605kg of I-methyl intermediate and 1,200kg of benzene into a 5000L enamel kettle, heat and stir at 60°C, control the amount of chlorine gas 590kg through the mass flow meter, and control the liquid chromatography of I-methyl intermediate in the total material in the heat preservation The content is less than 1%. The solvent is recovered by precipitation and the by-product hydrochloric acid is recovered by negative pressure to obtain the crude product of I-trichlorobenzyl intermediate. The by-product hydrochloric acid is recovered by solvent washing and liquid separation. The recovery rate of solvent dehydration is 92%, and the by-product 28% hydrochloric acid is 1050kg .

[0027] Under the protection of nitrogen, 1500 kg of dichloroethane and 310 kg of sulfonamide intermediates were sequentially added to the above-mentioned 5000L reaction kettle, stirred evenly and then raised to a reflux temperature of 90°C; T...

Embodiment 3

[0028] (Example 3) One-pot method does not separate and synthesize saflufenacil

[0029] Preparation of the target product in a small test:

[0030] Put 60.5g (0.20mol) of I-methyl intermediate and 100g of benzene into a 500mL glass bottle, heat and stir at 60°C, control the amount of chlorine gas 60g through the mass flow meter, and control the amount of I-methyl intermediate in the total material during the heat preservation The normalized content of liquid chromatography was less than 1%, and hydrogen chloride was pulled out under negative pressure to recover 90 g of by-product hydrochloric acid to obtain a crude benzene solution of I-trichlorobenzyl intermediate, which was directly used in the next step.

[0031] Under the protection of nitrogen, add 30.5g of sulfonamide intermediate to the above-mentioned 500mL reaction vessel in turn, stir well and then rise to the reflux temperature of 90°C; at this temperature, reflux and keep warm until the liquid phase of the I-trich...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to the technical field of herbicide manufacture, and discloses a preparation method of saflufenacil. In an organic solvent, the product benzene is obtained by using an I-methyl intermediate at a certain temperature through two-step reactions such as continuous chlorination and condensation. Flumesulam. The method of the invention has many sources of raw materials and obvious cost advantages, the preparation method is safer and more convenient, the total yield is high, and the three wastes are less. Only the by-product hydrochloric acid reduces a large amount of industrial salt solid waste, which is beneficial to industrialization.

Description

technical field [0001] The invention relates to the technical field of herbicide manufacture, in particular to a preparation method of saflufenacil. Background technique [0002] Safluefenacil is a uracil herbicide developed and developed by BASF. It can effectively control more than 70 kinds of weeds in corn, sorghum, soybean, small grains, cotton, fruit trees and nuts, and is very harmful to crops. Safe, with low volatility, "favorable" toxicological and ecological properties. Listed in 2009, the trade name is Babaijin. There are mainly two kinds of synthetic methods reported in the literature: one is the condensation of acid intermediates and sulfonamides under the conditions of condensing agents, resulting in more three wastes and many impurities in side reactions, especially the by-products of condensing agents are difficult to separate and reuse The second is to use acid chloride intermediates and sulfonamides to condense under acid-binding agent conditions. The proc...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/54
CPCC07D239/54
Inventor 刘长生肖石基
Owner 江苏乾元生物科技有限公司