HRID380444
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
Benzyl alcohol (215 mg, 1.99 mmol) was added to sodium hydride (0.017 g, 0.71 mmol) in anhydrous DMSO (0.4 ml). After 1 h ‘DABCO-purine’ (0.10 g, 0.36 mmol) was added and the reaction stirred for 48 h at room temperature. Acetic acid (0.06 ml) was added and the solvents removed in vacuo. The residue was purified by flash column chromatography on silica gel, eluting with 10% methanol in dichloromethane. The title compound was collected as a white solid (69 mg, 81%). λmax (CH3OH)/nm 285; δH (200 MHz, d6-DMSO) 7.96 (1H, s, C(8)H), 7.40 (5H, m, Ph), 6.44 (2H, s, NH2), 5.61 (2H, s, OCH2).
WORKUP
后处理
- customthe solvents removed in vacuo
- customThe residue was purified by flash column chromatography on silica gel
- washeluting with 10% methanol in dichloromethane
- customThe title compound was collected as a white solid (69 mg, 81%)