反应详情

A mixture of tert-butyl 2-[(3-amino-5,6-dimethyl-2-phenoxypyridin-4-yl)amino]ethylcarbamate (43.7 g, 117 mmol), triethyl orthoacetate (22.6 mL; 123 mmol), pyridine hydrochloride (4.4 g) and toluene (440 mL) was heated at reflux for 30 minutes. The reaction mixture was concentrated under reduced pressure to provide a brown oil. The oil was dissolved in ethyl acetate (1 L) and washed with water (2×500 mL). The aqueous washes were combined and extracted with ethyl acetate (2×500 mL). The combined organics were washed with brine, dried over magnesium sulfate and then concentrated under reduced pressure to provide 46.4 g of tert-butyl 2-(2,6,7-trimethyl-4-phenoxy-1H-imidazo[4,5-c]pyridin-1-yl)ethylcarbamate as a white solid, m.p. 180-182° C.

1. temperaturewas heated
2. temperatureat reflux for 30 minutes
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. customto provide a brown oil
5. washwashed with water (2×500 mL)
6. extractionextracted with ethyl acetate (2×500 mL)
7. washThe combined organics were washed with brine
8. dry with materialdried over magnesium sulfate
9. concentrationconcentrated under reduced pressure