HRID380444

反应详情

EQUATION

反应方程式

HRID 380444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customthe solvents removed in vacuo
  2. customThe residue was purified by flash column chromatography on silica gel
  3. washeluting with 10% methanol in dichloromethane
  4. customThe title compound was collected as a white solid (69 mg, 81%)