反应详情

温度

130 °C

48% Hydrobromic acid (10 mL) was added to 6-bromo-1-{3-fluoro-4-[(phenylmethyl)oxy]phenyl}-4-(methyloxy)-1H-indazole (D9) (1.16 g, 2.71 mmol) and the mixture heated at 130° C. for 3 hours. After cooling to room temperature, the mixture was diluted with ethyl acetate and water. The pH was adjusted to 7 by the addition of 2M aqueous sodium hydroxide solution. After separation of the organic layer, the aqueous phase was re-extracted with ethyl acetate. The combined organic layers were dried over magnesium sulphate, filtered and concentrated. The crude product was purified by silica gel chromatography eluting with 5-100% ethyl acetate in hexane. The product was further purified by MDAP to yield the title compound (E5) (170 mg).

1. temperatureAfter cooling to room temperature
2. customAfter separation of the organic layer
3. extractionthe aqueous phase was re-extracted with ethyl acetate
4. dry with materialThe combined organic layers were dried over magnesium sulphate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude product was purified by silica gel chromatography
8. washeluting with 5-100% ethyl acetate in hexane
9. customThe product was further purified by MDAP