Potassium Carbonate → 3-fluoro-4-[2-phenyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrrolo[2,3-b]pyridin-4-yloxy]-phenyl-carbamic acid t-butyl ester

温度

110 °C

4-Chloro-2-phenyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrrolo[2,3-b]pyridine (312 mg, 0.87 mmol) and (3-fluoro-4-hydroxy-phenyl)-carbamic acid t-butyl ester (336 mg, 1.48 mmol) were dissolved in anhydrous toluene (5 mL) under nitrogen atmosphere. After adding dicyclohexyl-phosphino-2,4,6-triisopropylbiphenyl (41 mg, 0.087 mmol), Pd2 dba3 (40 mg, 0.044 mmol) and potassium carbonate, the mixture was heated at 110° C. The resulting reaction mixture was cooled to room temperature and filtered by passing through a celite pad. The filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (hexane: ethyl acetate=9:1) to give the target compound as a white solid (404 mg, 0.73 mmol, 84% yield).

1. customThe resulting reaction mixture
2. temperaturewas cooled to room temperature
3. filtrationfiltered
4. concentrationThe filtrate was concentrated under reduced pressure
5. customThe resulting residue was purified by silica gel chromatography (hexane: ethyl acetate=9:1)

ORDレコード

ord-31bfbbe594f647fd980865b2eeb8dafe

出典データセット

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08957102B2