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Method for preparing m-carboxyl benzenesulfonic acid

A technology of carboxybenzenesulfonic acid and sodium benzenesulfonate, which is applied in the preparation of sulfonic acid and organic chemistry, and can solve the problems of long reaction time and large environmental pollution

Inactive Publication Date: 2011-06-15
深圳万乐药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] When m-carboxybenzenesulfonyl chloride is used, it needs to be temporarily synthesized, and the acylating reagent for preparing m-carboxybenzenesulfonyl chloride is large to environmental pollution; in addition, the synthesis of m-carboxybenzenesulfonic acid is actually a two-step reaction by the above method, and the reaction time is longer

Method used

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  • Method for preparing m-carboxyl benzenesulfonic acid
  • Method for preparing m-carboxyl benzenesulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 50 grams of sodium m-carboxybenzenesulfonate, 100 milliliters of hydrochloric acid and 100 milliliters of water into the reaction flask, stir at reflux for 2 hours, evaporate the solvent to dryness; add 400 milliliters of acetone to the residue, stir for 20 minutes, filter, and evaporate the filtrate to dryness; Add 400 ml of acetone, stir for 20 minutes, filter, and evaporate the filtrate to dryness; add 200 ml of acetone to the residue, stir for 20 minutes, filter, and evaporate the filtrate to dryness. The product was dried under vacuum at 90°C for 6 hours to obtain 35 g. Yield: 78.3%, moisture: 0.53%, melting point: 134.6-136.4°C.

Embodiment 2

[0016] Add 50 grams of sodium m-carboxybenzenesulfonate, 100 milliliters of concentrated hydrochloric acid and 100 milliliters of water into the reaction flask, reflux and stir for 2 hours, evaporate the solvent to dryness, add 400 milliliters of 1,4-dioxane to the residue, and stir for 20 minutes. Filter, and evaporate the filtrate to dryness; add 400 ml of 1,4-dioxane to the residue and stir for 20 minutes, filter, and evaporate the filtrate to dryness; add 200 ml of 1,4-dioxane to the residue, stir for 20 minutes, filter, and the filtrate Evaporate to dryness. The product was dried under vacuum at 90°C for 6 hours to obtain 32 g. Yield: 71.6%, moisture content: 0.62%, melting point: 134.4-136.3°C.

Embodiment 3

[0018] Add 50 grams of sodium m-carboxybenzenesulfonate, 100 milliliters of hydrochloric acid and 100 milliliters of water into the reaction flask, stir at reflux for 2 hours, evaporate the solvent to dryness; add 400 milliliters of tetrahydrofuran to the residue, stir for 20 minutes, filter, and evaporate the filtrate to dryness; Add 400 ml of tetrahydrofuran, stir for 20 minutes, filter, and evaporate the filtrate to dryness; add 200 ml of tetrahydrofuran to the residue, stir for 20 minutes, filter, and evaporate the filtrate to dryness. The product was dried under vacuum at 90°C for 6 hours to obtain 30 g. Yield: 67.1%, moisture: 0.78%, melting point: 134.1-136.2°C.

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Abstract

The invention discloses a process method for preparing m-carboxyl benzenesulfonic acid. In the process method, the m-carboxyl benzenesulfonic acid is prepared by reacting carboxyl sodium benzenesulfonate with hydrochloric acid and water. The synthesis method is low in equipment requirement, is simple in operation and is small in environment pollution, and can be produced in large scale.

Description

technical field [0001] The invention relates to the field of chemical pharmacy, in particular to a process for preparing m-carboxybenzenesulfonic acid. Background technique [0002] Although m-carboxybenzenesulfonic acid is an important pharmaceutical intermediate, it has been difficult to find a simple and practical synthetic method. U.S. Patent US 5387711 can be prepared by reacting m-carboxybenzenesulfonyl chloride with water. The reaction formula is as follows: [0003] [0004] When m-carboxybenzenesulfonyl chloride is used, it needs to be temporarily synthesized, and the acylating reagent for preparing m-carboxybenzenesulfonyl chloride is large to environmental pollution; in addition, the synthesis of m-carboxybenzenesulfonic acid is actually a two-step reaction by the above method, and the reaction time is longer. Contents of the invention [0005] The technical problem to be solved by the present invention is to provide a method that is simple, has little envir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/30C07C303/02
Inventor 钱建彬秦怀伟朱勇刘立力张广明井绪文
Owner 深圳万乐药业有限公司