反应详情

温度

170 °C

To 2-(difluoro(5-fluoropyridin-2-yl)methyl)-7-methylquinazolin-4-ol (413 mg, 1.35 mmol) were added Lawesson's reagent (820 mg, 2.03 mmol) and pyridine (3.5 mL), and the mixture was heated at 170° C. in a microwave reactor for 20 min. The mixture was partitioned between EtOAc (30 mL) and saturated aq NaHCO3 (50 mL), and the separated aqueous phase was extracted with EtOAc (2×30 mL). The combined organic layers were washed with 2N HCl and brine, dried over Na2SO4, and concentrated under reduced pressure onto Celite. The mixture was purified by silica get chromatography eluting with 0-30% EtOAc/hexanes to afford 2-(difluoro(5-fluoropyridin-2-yl)methyl)-7-methylquinazoline-4-thiol as an impure mixture (0.249 g). LCMS (ESI) m/z 322 (M+H)+.

1. customThe mixture was partitioned between EtOAc (30 mL) and saturated aq NaHCO3 (50 mL)
2. extractionthe separated aqueous phase was extracted with EtOAc (2×30 mL)
3. washThe combined organic layers were washed with 2N HCl and brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under reduced pressure onto Celite
6. customThe mixture was purified by silica
7. customget chromatography
8. washeluting with 0-30% EtOAc/hexanes