反应详情

To a solution of 10-amino-2-(5-(4-fluorobenzyl)-1,3,4-oxadiazol-2-yl)-3-hydroxy-7,8,9,10-tetrahydro-7,10-ethanopyrimido[1,2-a]azepin-4(6H)-one, Intermediate 12 (20 mg, 0.042 mmol) in DMF (1.5 mL) was added 2-(dimethylamino)-2-oxoacetic acid (9.79 mg, 0.084 mmol), N,N-dissopropylethylamine (0.044 mL, 0.251 mmol), HATU (31.8 mg, 0.084 mmol) and DMAP (5.11 mg, 0.042 mmol) and the resulting mixture stirred at room temp for 3 h and then purified by preparative HPLC to afford the title compound (5 mg, 9.47 μmol, 22.64% yield) as a purple solid. 1H NMR (500 MHz, CDCl3) δ ppm 11.10 (1H, br. s.), 9.60 (1H, s), 7.54 (2H, dd, J=8.39, 5.34 Hz), 7.10 (2H, t, J=8.55 Hz), 4.35 (2H, s), 4.24 (2H, br. s.), 3.44 (3H, s), 3.13 (3H, s), 2.99-3.08 (3H, m), 2.54 (1H, br. s.), 2.03-2.13 (2H, m), 1.85-1.94 (2H, m), 1.72-1.81 (2H, m). LCMS (M+H)+=497.18.

1. custompurified by preparative HPLC