反应详情

A solution of Example 1D (50 mg, 0.12 mmol), 2-aminonorbornane hydrochloride (106 mg, 0.58 mmol), and triethylamine (0.08 ml, 0.58 mmol) in DMF (2 mL) were heated to 120° C. in a sealed vial with shaking for 16 hours, then concentrated. The concentrate was dissolved in 1:1/DMSO:methanol (1.0 ml) and purified by reverse phase preparative HPLC with 0.1% TFA in H2O/CH3CN to provide the desired product. MS (APCI(+)) m/e 510 (M+H)+; 1H NMR (500 MHz, DMSO-d6) δ 12.45 (br s, 1H), 8.67 (d, 1H), 8.48 (d, 1H), 7.99 (dd, 1H), 7.95 (d, 2H), 7.78 (2d, 4H), 7.32 (t, 2H), 7.24 (d, 1H), 4.04 (m, 1H), 2.58 (m, 1H), 2.27 (m, 1H), 2.24-2.21 (m, 1H), 1.59-1.29 (m, 6H), 0.97 (dt, 1H).

1. concentrationconcentrated
2. dissolutionThe concentrate was dissolved in 1:1/DMSO
3. custommethanol (1.0 ml) and purified by reverse phase preparative HPLC with 0.1% TFA in H2O/CH3CN