反应详情

A mixture of Example 797A (0.09 g, 0.53 mmol) and POCl3 (0.244 g, 1.6 mmol) in toluene (5 mL) was heated under reflux for 3 hours. After reaction mixture cooled to room temperature, it was poured onto water and separated. The organic layer was dried over MgSO4 and concentrated. The residue was purified by silica gel column chromatography eluting with 100% EtOAc to give 0.072 g of the title compound (90%). MS (APCI) m/e 153 (M+H)+, 1H NMR (500 MHz, DMSO-d6): □ 8.51 (s, 1H), 8.36 (d, J=7.06 Hz, 1H), 7.45 (s, 1H), 6.97 (d, J=7.06 Hz, 1H), 6.67 (m, 1H).

1. temperatureunder reflux for 3 hours
2. customAfter reaction mixture
3. additionit was poured onto water
4. customseparated
5. dry with materialThe organic layer was dried over MgSO4
6. concentrationconcentrated
7. customThe residue was purified by silica gel column chromatography
8. washeluting with 100% EtOAc