23899-79-8Relevant articles and documents
Preparation method of theobromine
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Paragraph 0036-0053, (2021/01/11)
The invention discloses a preparation method of theobromine, and relates to the technical field of preparation of heterocyclic compounds containing purine ring systems. The method comprises the following steps: adding oxalyl chloride into cyanoacetic acid and a solvent at the temperature of -10-20 DEG C, concentrating to remove the solvent and oxalyl chloride after reaction, adding monomethylureaand the solvent at the temperature of 0-30 DEG C, adding alkali as an acid-binding agent, adding water after reaction, stirring, and filtering to obtain monomethyl cyanoacetylurea; adding water to dissolve cyanuric chloride, adding liquid caustic soda to adjust the pH value to 8-11, and reacting at 80-100 DEG C to generate methyl 4AU; dissolving monomethyl 4AU in formic acid, adding sodium nitrite, reacting at room temperature, adding a catalyst, keeping the temperature at 30-70 DEG C, recovering the catalyst after the reaction is finished, and concentrating mother liquor to recover formic acid, thereby obtaining monomethyl FAU; adding water and liquid caustic soda into monomethyl FAU, carrying out ring-closure reaction, and then adding acid to adjust to be neutral, so as to obtain 3-methyl xanthine; and carrying out a methylation reaction on 3-methylxanthine, and refining to obtain theobromine. The method has the advantages of few reaction steps, few side reactions, high yield and stable product quality.