反应详情

温度

150 °C

N-[4-(2,6,7-trimethyl-4-phenoxy-1H-imidazo[4,5-c]pyridin-1-yl)butyl]methanesulfonamide (4.20 g, 10.4 mmol) and ammonium acetate (42 g) were combined and then heated in a sealed tube at 150° C. for 36 hrs. The reaction mixture was allowed to cool and then it was dissolved in chloroform. The solution was extracted with 10% aqueous sodium hydroxide solution. The aqueous layer was separated and then extracted multiple times with chloroform. The organic layers were combined, dried over magnesium sulfate and then concentrated under reduced pressure to provide a yellow oil. The oil was dissolved in methanol and combined with 1M hydrochloric acid in diethyl ether (10.4 mL). The resulting white precipitate was isolated by filtration and dried. The solid was dissolved in water and the solution was adjusted to pH 10 with solid sodium carbonate. The resulting white precipitate was isolated by filtration, washed with diethyl ether and then dried in a vacuum oven at 80° C. to provide 2.00 g of N-[4-(4-amino-2,6,7-trimethyl-1H-imidazo[4,5-c]pyridin-1-yl)butyl]methanesulfonamide, m.p. 228–230° C.

1. temperatureto cool
2. extractionThe solution was extracted with 10% aqueous sodium hydroxide solution
3. customThe aqueous layer was separated
4. extractionextracted multiple times with chloroform
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customto provide a yellow oil
8. customThe resulting white precipitate was isolated by filtration
9. customdried
10. dissolutionThe solid was dissolved in water
11. customThe resulting white precipitate was isolated by filtration
12. washwashed with diethyl ether
13. customdried in a vacuum oven at 80° C.