HRID271268
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
An ice-cold solution of 2,6-dichloro-1H-purine (1.89 g, 10 mmol) in THF (10 mL) was treated with NaH (60% in oil, 440 mg, 11 mmol), stirred at 0° C. for 30 min, treated with ethyl bromoacetate (1.22 mL, 11 mmol), stirred at room temperature for 2 h, poured into sat. NaHCO3, extracted with EtOAc and the combined organic phase dried (MgSO4), concentrated in vacuo and purified by chromatography [SiO2; Heptane:EtOAc (2:1)] to give the title compound (1.46 g, 53%) as a white solid: IR νmax (Nujol)/cm−1 3106, 2985, 2955, 2924, 2854, 1734, 1598, 1557, 1374, 1341, 1298, 1156 and 884; NMR δH (400 MHz, CDCl3) 1.31 (3H, t, J7.0 Hz), 4.29 (2H, q, J7.0 Hz), 5.01 (2H, s), 8.17 (1H, s).
WORKUP
后处理
- stirringstirred at room temperature for 2 h
- extractionextracted with EtOAc
- dry with materialthe combined organic phase dried (MgSO4)
- concentrationconcentrated in vacuo
- custompurified by chromatography [SiO2; Heptane:EtOAc (2:1)]