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Synthesis technology of o-tolylthiourea

A technology of o-tolylthiourea and synthesis process, which is applied in the direction of organic chemistry, can solve the problems of high cost and long reaction time, and achieve the effects of high raw material utilization rate, high product yield and cost reduction

Inactive Publication Date: 2018-04-20
南京工业大学连云港工业技术研究院
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Problems solved by technology

The traditional preparation method of o-tolylthiourea is: react with o-toluidine and thiocyanate in an inert liquid (such as toluene) to prepare o-tolylthiourea, because the raw materials are easy to get, the reaction steps are few, and the conditions are easy to control Such advantages are adopted by industrial production, but there are disadvantages such as high cost and long reaction time (reference: Chen Tianyun, Sun Rongkang. Research on the synthesis process of N-o-tolylthiourea [J]. Fine Chemical Industry, 1993 (3): 35-38 .)

Method used

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  • Synthesis technology of o-tolylthiourea
  • Synthesis technology of o-tolylthiourea

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Experimental program
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Embodiment 1

[0024] Weigh 100.0g of o-toluidine, 100.0g of ammonium thiocyanate, and 500ml of deionized water into the reaction kettle, start stirring, weigh 14.0g of concentrated sulfuric acid, slowly add it to the reaction kettle, and simultaneously turn on the condensed water to control the temperature. After heat preservation at 65° C. for 1 h, the temperature was raised to 100° C. for 8 h. After the reaction, the temperature was lowered to room temperature, suction filtered, centrifuged and dried to obtain the final product. The product yield reaches 79.2%. The waste water produced by suction filtration separation is passed through a thin-film evaporator to evaporate salt (the steamed water continues to be used mechanically), after cooling down, centrifuge and dry to obtain by-product ammonium sulfate; the o-methylphenylthiourea obtained by suction filtration separation, Dry in a flash dryer for later use.

Embodiment 2

[0026] Weigh 100.0g of o-toluidine, 120.0g of ammonium thiocyanate, and 500ml of deionized water into the reactor, start stirring, weigh 15.4g of concentrated sulfuric acid, slowly add it into the reactor, and turn on the condensed water to control the temperature. After incubating at 65° C. for 1 h, the temperature was raised to 110° C. for 8 h. After the reaction, the temperature was lowered to room temperature, suction filtered, centrifuged and dried to obtain the final product. The product yield reaches 86.7%.

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Abstract

The invention discloses a synthesis technology of o-tolylthiourea. According to the invention, water is a reaction solvent, concentrated sulfuric acid is a catalyst, thiocyanate and o-tolylthiourea are raw materials, and a primary charging method is employed for synthesizing the o-tolylthiourea. The synthesis technology abandons usage of an organic solvent during a traditional technology, water istaken as the solvent, environment pollution is reduced, and cost is reduced; an one-step method is employed for synthesizing the o-tolylthiourea, raw material utilization rate is high, and operationis simple; factors of raw material ratio, solvent usage amount, concentrated sulfuric acid amount, temperature and time can be optimized, technical condition is mild, product yield is high, the synthesis technology has good economic benefit and social benefit, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a synthesis process of o-tolylthiourea, in particular to a synthesis process of o-tolylthiourea using water as a solvent. Background technique [0002] O-tolylthiourea is an important intermediate in the synthesis of the benzothiazole insecticide "tricyclazole", which is widely used both internationally and domestically. The traditional preparation method of o-tolylthiourea is: react with o-toluidine and thiocyanate in an inert liquid (such as toluene) to prepare o-tolylthiourea, because the raw materials are easy to get, the reaction steps are few, and the conditions are easy to control Such advantages are adopted by industrial production, but there are disadvantages such as high cost and long reaction time (reference: Chen Tianyun, Sun Rongkang. Research on the synthesis process of N-o-tolylthiourea [J]. Fine Chemical Industry, 1993 (3): 35-38 .). Contents of the invention [0003] The purpose of the present invention is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C335/16
CPCC07C335/16
Inventor 刘小祥王倩孙海超
Owner 南京工业大学连云港工业技术研究院