反应详情

温度

55 °C

To a solution of benzyl{[trans-4-(8-chloroimidazo[1,5-a]pyrazin-3-yl)cyclohexyl]methyl}carbamate (1.49 g, 0.00374 mol) in DMF (0.6 mL) was added NIS (1.0 g, 0.0045 mol). The reaction mixture was stirred at 55° C. overnight then diluted with EtOAc (20 mL), washed with water (2×40 mL) and brine (20 mL), then dried over Na2SO4 and concentrated in vacuo. The crude mixture thus isolated was chromatographed over silica gel eluting with hexane→hexane:EtOAc 1:1 to afford 1.7 g of the title compound. MS (ES+): m/z 525.01 [MH+].

1. washwashed with water (2×40 mL) and brine (20 mL)
2. dry with materialdried over Na2SO4
3. concentrationconcentrated in vacuo
4. customThe crude mixture thus isolated
5. customwas chromatographed over silica gel eluting with hexane→hexane:EtOAc 1:1