HRID373904

反应详情

EQUATION

反应方程式

HRID 373904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

9-[4-(Diethoxyphosphoryl)butoxy]guanine (0.12 g, 0.33 mmol) and bromotrimethylsilane (0.43 ml, 3.3 mmol) were dissolved in dimethylformamide (5 ml) and the reaction mixture was stirred at 23° C. for 3 hr. The solvent was evaporated under vacuum and the residue dissolved in methanol:water solution (9:1). The pH of the resulting solution was adjusted to 7.0 with diluted aq. ammonia and the solvents were evaporated to dryness. The product was purified by reversed phase chromatography (eluted with water) to give the title compound (65 mg, 64%) m.p. 208° C. (water), as its ammonium salt. 1H NMR: δH ((CD3)2, SO+D2O) 1.40 (2H, m, CH2P), 1.68 (4H, br.s, CH2CH2), 4.21 (2H, m, NOCH2), 7.89 (1H, s, H-8).

WORKUP

后处理

  1. customThe solvent was evaporated under vacuum
  2. dissolutionthe residue dissolved in methanol
  3. customthe solvents were evaporated to dryness
  4. customThe product was purified by reversed phase chromatography (eluted with water)