HRID1421238

反应详情

EQUATION

反应方程式

HRID 1421238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirring solution of 3-(2-furylmethyl)-8-methylxanthine (1.35 g, 5.48 mmol) in dimethyl sulfoxide (20 ml) was added sodium hydride (132 mg, 5.48 mmol) in one portion. After 30 minutes, chloromethyl pivalate (0.83 ml, 5.76 mmol) was added neat. The reaction was allowed to stir at ambient temperature for 24 h. The reaction was quenched by slow addition of water (75 ml). After stirring for 3 hours, the solid was filtered and rinsed with water (4×50 ml) and ethanol (50 ml). The product was recrystallized from ethanol/ethyl acetate/hexane to give 3-(2-Furylmethyl)-7-pivaloyloxymethyl-8-methylxanthine (1.36 g, 69%) as an off-white solid.

WORKUP

后处理

  1. customThe reaction was quenched by slow addition of water (75 ml)
  2. stirringAfter stirring for 3 hours
  3. filtrationthe solid was filtered
  4. washrinsed with water (4×50 ml) and ethanol (50 ml)
  5. customThe product was recrystallized from ethanol/ethyl acetate/hexane