反应详情

To a solution of 3-fluoro-4-[2-phenyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrrolo[2,3-b]pyridin-4-yloxy]-phenyl-carbamic acid t-butyl ester in methanol, a 1:1 solution (10 mL) of hydrochloric acid and methanol was added. The mixture was stirred at room temperature for 4 hours. The resulting reaction mixture was concentrated under reduced pressure and ether was added to the resulting residue. After stirring for 2 hours, the produced solid was collected by filtering. Thus obtained hydrochloride was dissolved in water and neutralized to about pH 8 by adding 1 M sodium hydroxide aqueous solution. The resulting mixture was extracted with ethyl acetate. The organic layer was separated and washed with sodium chloride aqueous solution. The organic layer was dried with Na2SO4 and then filtered. The filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (hexane:ethyl acetate=1:1) to give the target compound as a white solid (81 mg, 0.25 mmol, 40% yield).

1. customThe resulting reaction mixture
2. concentrationwas concentrated under reduced pressure and ether
3. additionwas added to the resulting residue
4. stirringAfter stirring for 2 hours
5. customthe produced solid was collected
6. filtrationby filtering
7. dissolutionThus obtained hydrochloride was dissolved in water and neutralized to about pH 8
8. additionby adding 1 M sodium hydroxide aqueous solution
9. extractionThe resulting mixture was extracted with ethyl acetate
10. customThe organic layer was separated
11. washwashed with sodium chloride aqueous solution
12. dry with materialThe organic layer was dried with Na2SO4
13. filtrationfiltered
14. concentrationThe filtrate was concentrated under reduced pressure
15. customThe resulting residue was purified by silica gel chromatography (hexane:ethyl acetate=1:1)