反应详情

温度

0 °C

To a cooled solution (0° C.) of 6-{4-[6-(3-chloro-4-fluoro-phenyl)-2-(2-methyl-pyrrolidin-1-yl)-pyrimidin-4-yl]-piperazin-1-yl}-5-methyl-pyridin-3-ylamine (146 mg, 0.30 mmol) in 10% H2SO4, add a solution of NaNO2 (22 mg, 0.32 mmol) in 3 mL H2O and stir at 0° C. for 30 min. Warm up to room temperature and heat at 90° C. for 1 h. Cool to room temperature, adjust pH to 7, and extract with EtOAc. Wash with brine, dry the solution (Na2SO4), and concentrate under reduced pressure. Purify the residue by flash column chromatography eluting with EtOAc:hexanes (1:1) to afford the title compound.

1. temperatureWarm up to room temperature
2. temperatureheat at 90° C. for 1 h
3. temperatureCool to room temperature
4. extractionextract with EtOAc
5. washWash with brine
6. dry with materialdry the solution (Na2SO4)
7. concentrationconcentrate under reduced pressure
8. customPurify the residue by flash column chromatography
9. washeluting with EtOAc:hexanes (1:1)