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レコード

ord-61b808fe928b4da6b9c84a5d04ed0bd0

出典データセット

uspto-grants-2004_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06797718B2