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N, N'-diisopropyl thiourea synthesis method

A technology of diisopropylthiourea and synthesis method, which is applied in the field of N, can solve problems such as expensive reagents, hidden dangers, and safety of poisonous gas leakage, and achieve the effects of simple feeding and post-processing, mild reaction conditions, and low pollution

Inactive Publication Date: 2007-05-16
ZHEJIANG UNIV
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  • Claims
  • Application Information

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Problems solved by technology

In addition, the application of this method will also produce a by-product - highly toxic gas hydrogen sulfide, which is very dangerous in the laboratory or in industry, and it is prone to poisonous gas leakage, which will cause great safety hazards
Moreover, in the preparation methods that have been reported, many experimental processes involve various problems such as strong acid or strong alkali conditions, expensive reagents, low yield, complicated post-treatment and long reaction time.

Method used

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  • N, N'-diisopropyl thiourea synthesis method
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  • N, N'-diisopropyl thiourea synthesis method

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preparation example Construction

[0014] N, the concrete reaction steps of the synthetic method of N '-diisopropylthiourea are as follows:

[0015] With water as the reaction solvent and PEG-400 as the catalyst, thiourea and diisopropylamine were refluxed at normal pressure for 20 to 36 hours, and then filtered and washed to obtain high-yield, high-purity N, N'-di Isopropylthiourea; reaction solvent and catalyst can be recycled. The molar equivalent ratio of thiourea and diisopropylamine is 0.4-0.6:1; the amount of catalyst PEG-400 is 2-10% molar equivalent of thiourea. The recommended reaction time is 24 to 30 hours; the recommended molar equivalent ratio of thiourea and diisopropylamine is 0.45 to 0.55:1, and the most preferred ratio is 0.5:1; the recommended dosage of catalyst PEG-400 is 2 to 7 times that of thiourea % molar equivalent, most preferably 4% molar equivalent.

Embodiment 1

[0018] Mix 10 millimoles of thiourea, 20 millimoles of diisopropylamine and 0.4 millimoles of PEG-400 in 20 milliliters of water, heat and reflux under normal pressure for 26 hours, finish the reaction, cool down, precipitate the product, filter (recover the filtrate), Washed with water and dried to obtain 1.4 g of N,N'-diisopropylthiourea with a yield of 78% and a melting point of 142-145°C.

Embodiment 2

[0020] 9 millimoles of thiourea and 20 millimoles of diisopropylamine were mixed in the filtrate that was recovered in Example 1, heated and refluxed at normal pressure for 36 hours, and the reaction was terminated, cooled, and the product was separated out, filtered (recovered from the filtrate), water After washing and drying, 1.42 g of N,N'-diisopropylthiourea was obtained, with a yield of 80% and a melting point of 143-145°C.

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Abstract

The invention discloses a synthesizing method of N, N'-diisopropyl thiourea, which comprises the following steps: adopting water as reacting solvent and 2-10% PEG-400 as catalyst; reacting thiourea and diisopropylamine with molar rate at 0.4-0.6: 1 under normal pressure to reflux for 20-36h; filtering; washing; separating to obtain the product.

Description

technical field [0001] The invention relates to a synthesis method of thiourea, in particular to a synthesis method of N, N'-diisopropylthiourea. Background technique [0002] N,N'-diisopropylthiourea is an important intermediate for the preparation of cefathiamidine and N,N'-diisopropylcarbodiimide (DCC). N, N'-Diisopropylcarbodiimide (DCC) is a low-temperature dehydrating agent commonly used in industries and laboratories to synthesize compounds such as aldehydes, ketones, polypeptides, anhydrides, and esters. It is widely used in fine chemicals such as medicine and pesticides. Industry: In industry, it is generally obtained by oxidizing N, N'-diisopropylthiourea with aqueous sodium hypochlorite solution. Therefore, how to synthesize N,N'-diisopropylthiourea more efficiently and greenly has attracted great attention. [0003] Many methods have been reported for the preparation of N,N'-diisopropylthiourea. Among them, a method for directly preparing N,N'-diisopropylthiou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C335/08
Inventor 沈阳林旭锋
Owner ZHEJIANG UNIV
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