404006-03-7Relevant articles and documents
Preparation method of thiourea alkylation derivative
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Paragraph 0037-0044; 0106-0110, (2021/03/31)
The invention discloses a preparation method of a thiourea alkylation derivative, which comprises the following steps: stirring an aldehyde, N-arylthiourea, trichlorosilane and Lewis base in an organic solvent at a range of -10 DEG C to room temperature for reaction, and carrying out after-treatment to obtain the thiourea alkylation derivative, wherein the molar ratio of the aldehyde to the N-arylthiourea is 1:2 to 2:1, the molar ratio of the aldehyde to the Lewis base is 1:(0.01-0.20), the molar ratio of the aldehyde to trichlorosilane is 1:(1-2), R1 is a C1-C5 saturated alkyl group, or an unsubstituted or substituted aromatic ring, and R2 is H, an electron withdrawing substituent or an electron donating substituent. According to the method, trichlorosilane is catalyzed by the micromolecular Lewis base, reductive alkylation of thiourea is realized, synthesis can be realized by a one-pot method, and the method is simple to operate, short in reaction time, low in substrate toxicity, lowin cost, easy to obtain, mild in reaction condition and high in safety.
Convenient synthesis of unsymmetrical N,N′-disubstituted thioureas in water
Li, Zhengyi,Chen, Yuan,Yin, Yue,Wang, Zhiming,Sun, Xiaoqiang
, p. 670 - 673 (2016/11/18)
A simple and convenient two-step method has been developed and used to synthesise 25 (4 of which are novel) unsymmetrical N,N′-disubstituted thioureas in water. Alkylamines or variously substituted arylamines reacted smoothly with phenyl chlorothionoformate at room temperature to form thiocarbamates, which were then reacted with another alkyl- or arylamine in water at reflux to afford the unsymmetrical N,N′-disubstituted thioureas in good to excellent yields. Mild conditions, simple work-up, high yields as well as using water as solvent are the major advantages of the method.