反应详情

温度

60 °C

Under inert atmosphere N-iodosuccinimide (3.6 g, 0.016 mol) and 3-(8-chloro-imidazo[1,5-a]pyrazin-3-yl)-1-hydroxymethyl-cyclobutanol (3.16 g, 0.012 mol) were dissolved in N,N-dimethylformamide (30 mL) and heated at 60° C. for 3.0 hours. The reaction mixture was then concentrated in vacuo to a dark oil and purified by HPFC Jones 20 g silica gel column, eluting with 5% MeOH: CH2Cl2 to yield a light brown fluffy solid which was triturated with diethyl ether and hexanes to afford the title compound; MS (ES+): m/z 379.85 (100) [MH+], 381.80 (30) [MH+++]; HPLC: tR=2.30 min (OpenLynx, polar—5 min).

1. concentrationThe reaction mixture was then concentrated in vacuo to a dark oil
2. custompurified by HPFC Jones 20 g silica gel column
3. washeluting with 5% MeOH
4. customCH2Cl2 to yield a light brown fluffy solid which
5. customwas triturated with diethyl ether and hexanes