反应详情

To a solution of compound 111 (39 mg, 0.08 mmol) in DMF (1.0 mL) was added ethylamine hydrochloride (20 mg, 0.08 mmol), FDPP (43 mg, 0.11 mmol), and DIEA (68 μL, 0.4 mmol). The flask was flushed with argon and the reaction mixture was stirred at RT for 72 h and then poured into a mixture of water (4 mL), HCl (4N, 2 mL), and EtOAc. The phases were separated. The organic phase was concentrated on silica in vacuo. The crude product was purified by chromatography eluting with EtOAc/petroleum ether (40-60) 50:50 to 100:0 as the eluent to afford the title compound as white foam. 13C NMR (DMSO-d6) δ 194.9, 164.8, 149.3, 145.2, 139.8, 135.9, 133.7, 133.7, 131.7, 128.2, 127.1, 126.6, 126.4 (dd), 125.0, 124.2 (dd), 123.0, 114.8, 111.9 (dd), 111.8, 105.0 (dd), 51.7, 33.6, 19.4, 14.4

1. customThe flask was flushed with argon
2. additionpoured into a mixture of water (4 mL), HCl (4N, 2 mL), and EtOAc
3. customThe phases were separated
4. concentrationThe organic phase was concentrated on silica in vacuo
5. customThe crude product was purified by chromatography
6. washeluting with EtOAc/petroleum ether (40-60) 50:50 to 100:0 as the eluent