反应详情

温度

120 °C

5-(3-Fluoro-4-hydroxyphenyl)-3-methyl-2-methylthio-3H-pyrimidin-4-one (Step 5, 0.39 g, 1.5 mmol) was suspended in 3.6 mL p-fluoroaniline and concentrated HCl (1 drop) was added. The reaction was heated in a microwave at 120° C. and 100 W for 10 min (using a Powermax feature on a CEM microwave). The reaction was cooled to RT and diluted with EtOAc (100 mL). The organic phase was extracted with 1 N NaOH (3×15 mL), and the aqueous extracts were neutralized with concentrated HCl. The aqueous layer was extracted with EtOAc (3×20 mL), and the organic extracts were combined, dried over Na2SO4, filtered, and concentrated to give desired compound. MS (ESI pos. ion) m/z: 330. Calc'd for C17H13F2N3O2: 329.10.

1. temperatureThe reaction was cooled to RT
2. extractionThe organic phase was extracted with 1 N NaOH (3×15 mL)
3. extractionThe aqueous layer was extracted with EtOAc (3×20 mL)
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated