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Production method for the intermediate methanesulfonic acid-2-propoxy ethyl ester of pretilachlor

A technology of methanesulfonic acid and propoxyethyl ester, which is applied in the production field of methanesulfonic acid-2-propoxyethyl ester, an intermediate of pretilachlor, can solve the complex recovery process, waste water need to be reprocessed, production Cost increase and other problems, to achieve the effect of high product content, less three wastes, and low cost

Inactive Publication Date: 2011-11-02
NANTONG WEILIKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of 2-propoxyethyl methanesulfonate produced by this method is relatively high, but an acid-binding agent is used in the intermediate process, which greatly increases the production cost
Although the acid-binding agent can be recovered, the recovery process is complicated and needs to be treated with alkali
During the recovery process of acid binding agent, there are a series of problems such as low recovery rate and reprocessing of waste water.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Put 104g of ethylene glycol n-propyl ether in a 500ml three-neck flask, add 123.5g of methanesulfonyl chloride and stir evenly. Add metal halide catalyst copper chloride (or copper bromide, ferric chloride or ferric bromide or other metal halide catalysts) 3g. Slowly heat up the temperature, absorb the tail gas with lye, heat to 130 ℃ for 2 hours, basically no bubbles are released. Sampling analysis: the content of 2-propoxyethyl methanesulfonate is 94.72%. 173g of product was obtained, and the yield was 95.12%.

Embodiment 2

[0014] Put 52g of ethylene glycol n-propyl ether in a 500ml three-neck flask, add 61.8g of methanesulfonyl chloride and stir evenly. Add catalyst iron chloride (or copper bromide, copper chloride or iron bromide or other metal halide catalyst) 1.5g. Slowly heat up the temperature, absorb the tail gas with lye, heat to 130 ℃ for 2.5 hours, basically no bubbles are released. Sampling analysis: the content of 2-propoxyethyl methanesulfonate was 94.44%. 87g of product was obtained, and the yield was 95.67%.

Embodiment 3

[0016] Put 208g of ethylene glycol n-propyl ether in a 1000ml three-neck flask, add 247g of methanesulfonyl chloride and stir evenly. Add catalyst copper chloride (or copper bromide, ferric chloride or ferric bromide or other metal halide catalysts) 6g. The reaction steps are the same as those in Examples 1 and 2. Sampling and analysis: the content of 2-propoxyethyl methanesulfonate is 95.10%. Obtain product 346g, yield is 95.07%.

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Abstract

The invention discloses a production method for the intermediate methanesulfonic acid-2- propoxy ethyl ester of pretilachlor. According to the method, glycol monopropyl ether reacts with methanesulfonyl chloride, and a metal halide is used as a catalyst for the reaction. The production method provided in the invention has the advantages of easy operation, simple equipment, a small amount of the three wastes (waste gas, waste water and industrial residue) and low cost, and the content and yield of the produced products are high.

Description

technical field [0001] The invention relates to a production method of pretilachlor intermediate methanesulfonate-2-propoxyethyl ester. Background technique [0002] The current domestic synthesis technology of pretilachlor intermediate methanesulfonate-2-propoxyethyl ester is generally as follows: a certain amount of ethylene glycol monopropyl ether and methylsulfonyl chloride (8% in excess) are mixed evenly, and the temperature is lowered to Below 10°C, slowly add triethylamine dropwise (other acid-binding agents are also reported). After the dropwise addition was completed, keep the temperature for 2 hours naturally. After the sampling is qualified, add water to wash it, and let it stand for stratification to obtain the target product. The yield of 2-propoxyethyl methanesulfonate produced by this method is relatively high, but an acid-binding agent is used in the intermediate process, which greatly increases the production cost. Although the acid-binding agent can be r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/66C07C303/28
Inventor 陈朋朋李国华章奉良李可庆
Owner NANTONG WEILIKE CHEM
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