反应详情

A solution of the intermediate from Step E in phosphoryl chloride (9.43 mL, 101 mmol) was heated at 105° C. for 30 min. The majority of the phosphoryl chloride was removed in vacuo. The crude product was partitioned between saturated aq. NaHCO3 and EtOAc. The aqueous layer was separated and further extracted with EtOAc (2×). The combined extracts were dried (Na2SO4) and concentrated in vacuo to give the desired product, as a yellow solid. 1H NMR (600 MHz, CHCl3-d) δ 8.47 (dd, J=7.1, 1.6 Hz, 1H); 8.41 (dd, J=3.8, 1.7 Hz, 1H); 6.98 (dd, J=7.1, 3.8 Hz, 1H); 3.35-3.31 (m, 2H); 2.68-2.57 (m, 2H). m/z=291.1 (M+H).

1. customThe majority of the phosphoryl chloride was removed in vacuo
2. customThe crude product was partitioned between saturated aq. NaHCO3 and EtOAc
3. customThe aqueous layer was separated
4. extractionfurther extracted with EtOAc (2×)
5. dry with materialThe combined extracts were dried (Na2SO4)
6. concentrationconcentrated in vacuo