反应详情

温度

0 °C

1,1,1,3,3,3-Hexafluoro-2-(4-(hydroxymethyl)-3-propylphenyl)propan-2-ol (0.474 mmol, 150 mg) was dissolved in dichloromethane (5 mL) and triethylamine (1.423 mmol, 144 mg) added. The mixture was cooled to 0° C. before the addition of methanesulfonyl chloride (0.611 mmol, 70.0 mg). The mixture was stirred at 0° C. for 90 min. The reaction mixture was diluted with dichloromethane (50 mL) and washed with water (2×10 mL). The organic phase was dried over magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure. The resulting residue was dissolved in acetonitrile (4 mL) and 1-(2-amino-2-methylpropyl)-3-(2-fluoro-4-(piperidin-4-ylmethyl)phenyl)urea (0.341 mmol, 110 mg) was added followed by potassium carbonate (1.023 mmol, 141 mg). The mixture was heated to reflux for 16 hours. The mixture was cooled, filtered and the filtrate was concentrated under reduced pressure. The resulting residue was purified by HPLC and treated with strong cation exchange column chromatography to afford the title compound (12 mg).

1. washwashed with water (2×10 mL)
2. dry with materialThe organic phase was dried over magnesium sulfate
3. filtrationfiltered
4. concentrationthe filtrate was concentrated under reduced pressure
5. dissolutionThe resulting residue was dissolved in acetonitrile (4 mL)
6. temperatureThe mixture was heated
7. temperatureto reflux for 16 hours
8. temperatureThe mixture was cooled
9. filtrationfiltered
10. concentrationthe filtrate was concentrated under reduced pressure
11. customThe resulting residue was purified by HPLC
12. additiontreated with strong cation exchange column chromatography