548-37-8Relevant articles and documents
Synthesis method and application of verbenalin
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Paragraph 0026; 0031-0034; 0039-0042; 0047-0050; 0055-0058, (2020/07/13)
The invention puts forward a synthesis method and application of verbenalin. A compound A, a compound B, triphenylphosphine and anhydrous tetrahydrofuran are mixed and are cooled to 0-10 DEG C; diethyl azodicarboxylate is dripped, and a room temperature is recovered; after reaction is carried out, system pH is regulated to 1; at a temperature of 40-50 DEG C, reaction is carried out for 5-10h; suction filtration is carried out, and a filter cake is washed; water is added to carry out stirring and dissolving, and then, suction filtration is carried out; filtrate pH is regulated to 10-12, methylene dichloride is added for extraction, and after a methylene dichloride phase is dried, purification is carried out to obtain a compound C; the compound C and absolute methanol are added into a reaction flask and are cooled to 0-5 DEG C; RhCl(PPh3)3 is added, and after rection is carried out for 20-40 min, recovering to the room temperature; reaction is continuously carried out for 2-6h, and filtering is carried out; after vacuum concentration is carried out, extraction and liquid division are carried out; and the methylene dichloride phase is dried, and column chromatography extraction is carried out to obtain the verbenalin. According to the method disclosed by the invention, the yielding capacity of the verbenalin is greatly improved, an impurity, i.e., hastatoside, can prevent from being introduced in a verbena officinalis L. extraction process, the synthesized verbena officinalis L. ingredient liquid glycoside has higher purity, and quality is better.