反应详情

tert-Butyl 4-ethyl-4-(5-oxopyrrolo[4,3,2-de][2,6]naphthyridin-4(1H,3H,5H)-yl)piperidine-1-carboxylate (50 mg, 0.124 mmol), HATU (94 mg, 0.248 mmol), and 4-dimethylaminopyridine (46 mg, 0.373 mmol) were stirred in DMF (3 mL) at room temperature for 1 h. The solution was concentrated in vacuo and dissolved in DCM (3 mL) and TFA (1 mL) and allowed to stir at room temperature for 1 h. The solution was concentrated in vacuo and was purified via preparative HPLC 10% to 30% B in A and gave 28 mg of the title compound as its TFA salt. 1H NMR (400 MHz, CD3OD) δ 7.36 (m, 1H), 7.27 (m, 1H), 5.04 (s, 2H), 3.22-3.34 (m, 2H), 3.19-3.21 (m, 2H), 2.95-2.98 (m, 2H), 2.13-2.23 (m, 4H), 0.97 (t, 3H, J=7.6 Hz). [M+H] found 285.

1. concentrationThe solution was concentrated in vacuo
2. dissolutiondissolved in DCM (3 mL)
3. concentrationThe solution was concentrated in vacuo
4. customwas purified via preparative HPLC 10% to 30% B in A