反应详情

温度

130 °C

A mixture of compound 17 (1.5 g, 3.7 mmol) and phenylphosphoro dichloridate (5 mL) was heated at 130° C. for 5 h. The reaction mixture was cooled to rt, diluted with cold water (10 mL), cooled to 0° C., quenched with saturated NaHCO3 solution and extracted with EtOAc (2×50 mL). The combined organic layer was washed with brine (50 mL), dried (Na2SO4) and evaporated. The crude compound was purified by trituration with EtOAc to obtain 18 (0.7 g, 46%) as a pale brown solid. Rf: 0.5 (10% MeOH/DCM); (m/z): 408 [M+1]+; 1H NMR (400 MHz, DMSO-d6): δ10.01 (1H, s), 9.40 (1H, d, J=2.4 Hz), 9.11 (1H, d, J=2.4 Hz), 8.85 (1H, d, J=2.4 Hz), 8.70 (1H, d, J=5.2 Hz), 8.21-8.18 (1H, dd, J=2.4, 8.8 Hz), 7.62 (1H, d, J=5.6 Hz), 7.40 (1H, d, J=8.4 Hz), 3.59-3.54 (6H, m), 2.46-2.41 (4H, m).

1. temperatureThe reaction mixture was cooled to rt
2. temperaturecooled to 0° C.
3. customquenched with saturated NaHCO3 solution
4. extractionextracted with EtOAc (2×50 mL)
5. washThe combined organic layer was washed with brine (50 mL)
6. dry with materialdried (Na2SO4)
7. customevaporated
8. customThe crude compound was purified by trituration with EtOAc