反应详情

Into a RBF 3-(8-chloro-1-iodo-imidazo[1,5-a]pyrazin-3-yl)-cyclobutanone (1.00 g, 0.0029 mol) and sodium triacetoxyborohydride (1.30 g, 0.006 mol) were dissolved in 1,2-dichloroethane (65.0 mL) and a solution of 1-acetylpiperazine (0.39 g, 0.003 mol) in 1,2-dichloroethane was added to the reaction. The reaction mixture was stirred at room temperature for 2 h. The crude product was concentrated in vacuo and the dissolved in CH2Cl2 (25.0 mL) and washed with saturated NaHCO3 solution (1×40 mL). The product was dried with sodium sulfate and concentrated in vacuo to yield a light yellow solid; MS (ES+): m/z 459.84 (100) [MH+], 461.80 (40) [MH+++]; HPLC: tR=1.81 min (OpenLynx, polar—5 min); 1H NMR (CDCl3, 400 MHz) δ 2.04-2.15 (m, 3 H) 2.26-2.50 (m, 6 H) 2.55-2.72 (m, 2 H) 2.83-2.99 (m, 1 H) 3.29-3.52 (m, 3 H) 3.56-3.67 (m, 2 H) 7.29 (d, 1 H) 7.58 (d, 1 H).

1. concentrationThe crude product was concentrated in vacuo
2. dissolutionthe dissolved in CH2Cl2 (25.0 mL)
3. washwashed with saturated NaHCO3 solution (1×40 mL)
4. dry with materialThe product was dried with sodium sulfate
5. concentrationconcentrated in vacuo
6. customto yield a light yellow solid
7. customMH+++]; HPLC: tR=1.81 min (OpenLynx, polar—5 min)