40371-21-9Relevant articles and documents
Preparation method of tetramisole intermediate hydroxysalt
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Paragraph 0017-0019; 0023; 0024-0026; 0029-0031, (2021/01/20)
The invention relates to a preparation method of a tetramisole intermediate hydroxysalt in the technical field of broad-spectrum anthelmintics. The method comprises the following steps of: adding an aprotic solvent, acetophenone and inorganic base into a reaction device, performing heating, and stirring the substances uniformly; then adding 2-chloroethylamine hydrochloride into the reaction devicein batches, continuously carrying out heat preservation reaction, performing cooling and filtering after the reaction is finished, and carrying out vacuum concentration on filtrate to remove the solvent to obtain an oily compound; and adding water and the oily compound into a reaction device, adjusting the pH value by using hydrochloric acid to dissolve and clarify the material, adding thiourea,performing heating, distilling and concentrating until the internal temperature reaches 108-110DEG C, further carrying out reflux reaction, conducting cooling, crystallizing and filtering after the reaction is finished, washing the filter cake by using 95% ethanol, further performing filtering and drying, and drying the solid to obtain the hydroxysalt. The yield of the hydroxysalt can reach 90% orabove, the purity can reach 99% or above, the content can reach 98% or above, the preparation is convenient, the process is simple, and the method is an alternative method for industrial production of the hydroxysalt and tetramisole.