反应详情

温度

90 °C

To a stirred solution of Intermediate 212C (95 mg, 0.509 mmol) in toluene (5 ml) was added TEA (0.118 mL, 0.848 mmol), DPPA (0.047 mL, 0.204 mmol) and the reaction mixture was stirred at 90° C. for 1 h. The reaction mixture was cooled RT and to it was added a solution of Intermediate 185B (50 mg, 0.170 mmol) in DMF (2 ml) and stirred at RT for 16 h. The reaction was quenched with a 10% aqueous solution of NaHCO3 and extracted with EtOAc (2×20 mL). The combined organic layer dried over Na2SO4, filtered and the filtrate evaporated. The crude compound was purified by preparative HPLC to afford Compound 212 as an off-white solid (6 mg, 7% yield). HPLC retention times 9.95 min. and 9.08 min. (Methods A and B respectively). MS(ES): m/z 478 [M+H]+; 1H NMR (400 MHz, MeOH-d1) δ ppm 7.75-7.77 (m, 1H), 7.58-7.62 (m, 1H), 7.29-7.33 (t, J=8.84 Hz, 1H), 4.85 (s, 2H), 4.23 (s, 2H), 4.18-4.21 (t, J=5.24 Hz, 2H), 3.90-3.92 (t, J=5.24 Hz, 2H), 1.37 (s, 6H).

1. temperatureThe reaction mixture was cooled RT and to it
2. stirringstirred at RT for 16 h
3. customThe reaction was quenched with a 10% aqueous solution of NaHCO3
4. extractionextracted with EtOAc (2×20 mL)
5. dry with materialThe combined organic layer dried over Na2SO4
6. filtrationfiltered
7. customthe filtrate evaporated
8. customThe crude compound was purified by preparative HPLC