反应详情

温度

55 °C

5-Aminopyrimidin-4,6-dithiol (Intermediate 41) (1.26 g) and 1-methyl-4-phenyl-1H-imidazole-5-carboxylic acid (Intermediate 3) (1.6 g) were dissolved/ suspended in pyridine (30 mL) and heated at 55° C. under an inert atmosphere. POCl3 (1.55 mL) was added dropwise over 5 minutes, after 2 hours the reaction mixture was concentrated in vacuo and 2M NaOH (15 mL) added cautiously. After stirring for 15 minutes, concentrated HCl was added to acidify to pH 5, the precipitated solid was filtered, washed with water (40 mL), diethyl ether (50 mL) then dried under high vacuum to give the title compound as a yellow solid (1.83 g, 71%);

1. concentrationwas concentrated in vacuo and 2M NaOH (15 mL)
2. additionadded cautiously
3. additionconcentrated HCl was added
4. filtrationthe precipitated solid was filtered
5. washwashed with water (40 mL), diethyl ether (50 mL)
6. customthen dried under high vacuum