Trimethyl orthoacetate → tert-butyl 2-[2-(2,6,7-trimethyl-4-phenoxy-1H-imidazo[4,5-c]pyridin-1-yl)ethoxy]ethylcarbamate

Trimethyl orthoacetate (3.55 mL, 28.27 mmol), tert-butyl 2-{2-[(3-amino-5,6-dimethyl-2-phenoxypyridin-4-yl)amino]ethoxy}ethylcarbamate (11.21 g, 26.92 mmol), pyridine hydrochloride (1.12 g) and toluene (120 mL) were combined and heated at reflux for 2.5 hours. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (300 mL), washed with water (3×100 mL) and brine (1×100 mL), dried over magnesium sulfate and then concentrated under reduced pressure to provide 9.85 g of tert-butyl 2-[2-(2,6,7-trimethyl-4-phenoxy-1H-imidazo[4,5-c]pyridin-1-yl)ethoxy]ethylcarbamate.

1. temperatureheated
2. temperatureat reflux for 2.5 hours
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. dissolutionThe residue was dissolved in ethyl acetate (300 mL)
5. washwashed with water (3×100 mL) and brine (1×100 mL)
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated under reduced pressure

ORD 기록

ord-66aab8edd9844eff9bcb9813f21a170c

출처 데이터셋

uspto-grants-2007_05

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07220758B2