乙腈 → Methyl 3-(4-{[(2R)-4-[5-fluoro-2-(methyloxy)phenyl]-2-hydroxy-4-methyl-2-(trifluoromethyl)pentyl]amino}-6-methyl-1H-indazol-1-yl)benzoate

温度

83 °C

(2R)-2-{2-[5-Fluoro-2-(methyloxy)phenyl]-2-methylpropyl}-2-(trifluoromethyl)oxirane (530 mg, 1.81 mmol) was added to acetonitrile (2.5 mL), followed by the addition of methyl 3-(4-amino-6-methyl-1H-indazol-1-yl)benzoate (590 mg, 2.1 mmol) and yttrium trifluoromethanesulfonate (197 mg, 0.37 mmol) at room temperature under a nitrogen atmosphere. The resulting mixture was then heated to reflux (83° C.) overnight, then allowed to cool down to room temperature and diluted with ethyl acetate (7 mL). The mixture was washed successively with saturated sodium bicarbonate (10 mL) and water (10 mL), dried and concentrated. The residue was then purified by column chromatography (10% ethyl acetate in cyclohexane) to give, after concentration, the title compound (540 mg).

1. temperatureThe resulting mixture was then heated
2. temperatureto cool down to room temperature
3. washThe mixture was washed successively with saturated sodium bicarbonate (10 mL) and water (10 mL)
4. customdried
5. concentrationconcentrated
6. customThe residue was then purified by column chromatography (10% ethyl acetate in cyclohexane)
7. customto give
8. concentrationafter concentration

ORD记录

ord-cdd28021731b454ea0f8b9960d2a1e18

来源数据集

uspto-grants-2012_05

DOI

10.6084/m9.figshare.5104873.v1

专利号

US08178573B2