反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
3-[2-(Furan-3-yl)pyrimidin-4-yl]-7-(1-methyl-1-triethylsilanyloxyethyl)imidazo[1,2-α]pyrimidine (203 mg, 0.47 mmol) in EtOH (10 ml) was treated with conc. HCl (15 drops) and the resulting solution was stirred at room temperature for 12 h during which time a precipitate formed. The solid was filtered off and was then partitioned between CH2Cl2 (20 ml) and NaHCO3 solution (20 ml). The organic layer was separated and the aqueous extracted with CH2Cl2 (3×20 ml). The combined organic extracts were dried (MgSO4) and concentrated under reduced pressure to afford 2-[3-(2-(furan-3-yl)pyrimidin-4-yl)imidazo[1,2-α]pyrimidin-7-yl]propan-2-ol (64 mg, 42%): 1H NMR (400 MHz, d6-DMSO) δ 10.29 (1H, d, J 7.3), 8.81 (1H, s), 8.77 (1H, d, J 5.4), 8.68 (1H, s), 7.89 (1H, d, J 5.4), 7.87 (1H, s), 7.74 (1H, d, J 7.3), 7.20 (1H, s), 5.61 (1H, s), 1.54 (6H, s); m/z (ES+) 322 (M+H+).
WORKUP
后处理
- customformed
- filtrationThe solid was filtered off
- customwas then partitioned between CH2Cl2 (20 ml) and NaHCO3 solution (20 ml)
- customThe organic layer was separated
- extractionthe aqueous extracted with CH2Cl2 (3×20 ml)
- dry with materialThe combined organic extracts were dried (MgSO4)
- concentrationconcentrated under reduced pressure