反应详情

温度

150 °C

A sealed tube containing ammonium acetate (7.5 g) and 2-butyl-6,7-dimethyl-4-phenoxy-1-(2-phenoxyethyl)-1H-imidazo[4,5-c]pyridine (0.75 g) from Part C was heated in an oil bath to 150° C. for 48 hours. The reaction reached 70% completion and was allowed to cool to room temperature. The reaction mixture was then dissolved in ethyl acetate and washed with a saturated aqueous solution of sodium bicarbonate. The organic layer was dried with magnesium sulfate and concentrated under reduced pressure. The product was passed through a silica gel column using 10/90 methanol/ethyl acetate as the eluant. To remove impurities, the product was recrystallized twice from acetonitrile with charcoal. The resulting white crystals were crushed and dried to yield 2-butyl-6,7-dimethyl-1-(2-phenoxyethyl)-1H-imidazo[4,5-c]pyridin-4-amine, m.p. 130.0–132.0° C.

1. temperatureto cool to room temperature
2. washwashed with a saturated aqueous solution of sodium bicarbonate
3. dry with materialThe organic layer was dried with magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customTo remove impurities
6. customthe product was recrystallized twice from acetonitrile with charcoal
7. customThe resulting white crystals were crushed
8. customdried