HRID1421238
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
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
- customThe reaction was quenched by slow addition of water (75 ml)
- stirringAfter stirring for 3 hours
- filtrationthe solid was filtered
- washrinsed with water (4×50 ml) and ethanol (50 ml)
- customThe product was recrystallized from ethanol/ethyl acetate/hexane