反应详情

温度

160 °C

Ammonium acetate (25 g) and 2,6,7-trimethyl-1-[5-(methylthio)pentyl]-4-phenoxy-1H-imidazo[4,5-c]pyridine (2.75 g, 7.45 mmol) were combined and heated at 160° C. overnight. The reaction mixture was cooled to 0° C. and then diluted with water (50 mL). The pH was adjusted to >13 with 15% sodium hydroxide and then the mixture was extracted with chloroform (2×100 mL). The combined extracts were dried over magnesium sulfate and then concentrated under reduced pressure. The residue was purified on deactivated silica gel (triethylamine) eluting with 2% methanol in chloroform and then recrystallized from ethyl acetate/hexanes to provide 1.089 g of 2,6,7-trimethyl-1-[5-(methylthio)pentyl]-1H-imidazo[4,5-c]pyridin-4-amine as an off white solid, m.p. 121–122° C.

1. temperatureThe reaction mixture was cooled to 0° C.
2. extractionthe mixture was extracted with chloroform (2×100 mL)
3. dry with materialThe combined extracts were dried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified on deactivated silica gel (triethylamine)
6. washeluting with 2% methanol in chloroform
7. customrecrystallized from ethyl acetate/hexanes