51672-22-1Relevant articles and documents
Preparation method of 2-methylamino-5-t-butyl-1,3,4-thiadiazole
-
Paragraph 0021-0032, (2019/02/04)
The invention relates to a preparation method of 2-methylamino-5-t-butyl-1,3,4-thiadiazole. The method comprises the following steps: adding 4-methylthiosemicarbazide and pivaloyl chloride into a reaction kettle, adding a first organic solvent, performing a reaction, heating the obtained solution, adding the dehydrating agent pivaloyl chloride again, carrying out a reaction for 1-3 h, cooling theobtained solution to 30-60 DEG C, filtering the cooled solution, and adding water to the obtained filtrate to obtain pivalic acid; and adding an alkali to a solid obtained by the filtration in order to adjust the pH value to 7-8, adding a second organic solvent, performing stirring, and carrying out reduced pressure distillation on the obtained organic phase to obtain the 2-methylamino-5-t-butyl-1,3,4-thiadiazole. The method has few side reactions, and the pivalic acid produced by the reaction can be used to further prepare pivaloyl chloride for reuse, so the method is in line with the development direction of modern green chemistry.
