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Synthetic method for chelating agent of 5-methyl-2-hydrosulfuryl benzoic acid

A technology of mercaptobenzoic acid and p-methylthiophenol, which is applied in the field of synthesizing 5-methyl-2-mercaptobenzoic acid, can solve the problems of deactivation of amino-type chelating agents, and achieve easy separation and purification, air stability, and reaction high efficiency effect

Inactive Publication Date: 2012-08-01
CHANGSHA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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Problems solved by technology

The above-mentioned chelating agents have great limitations in the treatment of heavy metal wastewater, and the dimercapto-type chelating agents are easy to release H under acidic conditions. 2 S, inactivated by oxidation to sulfoxide in air, and amino-type chelating agents are also easily oxidized to nitroso compounds by air and inactivated

Method used

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Embodiment Construction

[0010] Chloroform was dried over anhydrous magnesium sulfate and used after sublimation of anhydrous aluminum trichloride. Add 6 mL of chloroform and anhydrous aluminum trichloride dissolved in 0.62 g of p-methylthiophenol into a 100 mL three-necked flask, and stir at room temperature for 10 min. Add 0.47 mL of oxalyl chloride dropwise under stirring, and stir at room temperature for 2 hours after the dropwise addition is complete. Add 8 mL of 6mol / L hydrochloric acid for acidolysis, raise the temperature to 50°C and continue to stir until no HCl gas is released, separate the liquids after cooling, wash with water until neutral, take the lower layer solution and rotary evaporate to dryness, wash with water, wash with ethanol, wash with water again, and dry A yellow solid was obtained, which was recrystallized from chloroform and ethanol to obtain yellow 5-methyl-2-mercaptobenzoic acid crystals.

[0011] 1. a kind of method taking p-methylthiophenol as raw material synthetic 5...

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Abstract

The invention relates to a synthetic method for 5-methyl-2-hydrosulfuryl benzoic acid. The 5-methyl-2-hydrosulfuryl benzoic acid is a chelating agent; and reactants that are p-methyl thiophenol, catalytic agents (that can be aluminium chloride or iron trichloride) and oxalyl chloride are added in organic solvent (that can be petroleum ethers or ethers or methylene chloride or chloroform or chlorobenzene or nitrobenzene), so that 5-methyl-2-hydrosulfuryl benzoic acid is synthesized. The synthetic method achieves simple technology, products are easy to separate and purify, and the yield coefficient is high.

Description

[0001] The invention relates to a synthesis method of 5-methyl-2-mercaptobenzoic acid. This material is a kind of chelating agent, in organic solvent (can be sherwood oil, diethyl ether, dichloromethane, chloroform, chlorobenzene, nitrobenzene), add reactant p-methyl thiophenol, catalyst (can be Aluminum trichloride, ferric chloride) and oxalyl chloride, synthesized 5-methyl-2-mercaptobenzoic acid. The synthesis method has simple process, easy separation and purification of products, and high yield. [0002] A kind of method of synthesizing 5-methyl-2-mercaptobenzoic acid technical field [0003] The invention relates to a method for synthesizing 5-methyl-2-mercaptobenzoic acid, belonging to the technical field of fine chemical product production. technical background [0004] High-concentration heavy metal wastewater has serious harm to human health, living environment and ecological system. The "Mizugo disease" and "Itai-itai disease" that occurred in Japan have attracte...

Claims

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Application Information

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IPC IPC(8): C07C323/62C07C319/12C02F1/62C02F101/20
Inventor 湛雪辉李朝辉李侠姜红宇曹芬
Owner CHANGSHA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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