HRID448976
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 3-(8-chloro-1-iodoimidazo[1,5-a]pyrazin-3-yl)-1-hydroxymethylcyclobutanol (4.08 g, 0.011 mol) in THF (120 mL) and water (40 mL) was charged with sodium periodate (2.8 g, 0.013 mol) at 0° C. The reaction warmed to rt and stirred for 5 h. The reaction mixture was diluted with EtOAc and then washed with brine. The organic phase was dried over Na2SO4, filtered, and concentrated in vacuo to afford the title compound as a yellow solid; 1H NMR (CDCl3, 400 MHz) δ 7.56 (1H, d, J=4.94 Hz), 7.32 (1H, d, J=4.98 Hz), 3.64 (5H, m); MS (ES+): m/z 347.82 and 349.85 [MH+]; HPLC: tR=2.89 min. (OpenLynx, polar—5 min.).
WORKUP
后处理
- washwashed with brine
- dry with materialThe organic phase was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo