HRID328194
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
7.3 g. triacetyl-6-chloro-9-(β-D-ribofuranosyl)-purine, 2.1 g. methyl-but-2-enylamine and 2.8 ml. triethylamine were heated under reflux for 2 hours in 100 ml. isopropanol. After cooling, the reaction mixture was mixed with 200 ml. diethyl ether, extracted twice with water and the organic phase evaporated to dryness in a vacuum. The residue was dissolved in 100 ml. 25% methanolic ammonia and then left to stand overnight at ambient temperature. The solution was thereafter evaporated and the residue obtained was recrystallized from water. 4.1 g. (70% of theory) N(6)-methyl-N(6)-but-2-enyl-adenosine were obtained; m.p. 160° - 162° C.
WORKUP
后处理
- temperatureunder reflux for 2 hours in 100 ml
- temperatureAfter cooling
- additionthe reaction mixture was mixed with 200 ml
- extractiondiethyl ether, extracted twice with water
- customthe organic phase evaporated to dryness in a vacuum
- dissolutionThe residue was dissolved in 100 ml
- wait25% methanolic ammonia and then left
- customThe solution was thereafter evaporated
- customthe residue obtained
- customwas recrystallized from water