HRID328194

反应详情

EQUATION

反应方程式

HRID 328194 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureunder reflux for 2 hours in 100 ml
  2. temperatureAfter cooling
  3. additionthe reaction mixture was mixed with 200 ml
  4. extractiondiethyl ether, extracted twice with water
  5. customthe organic phase evaporated to dryness in a vacuum
  6. dissolutionThe residue was dissolved in 100 ml
  7. wait25% methanolic ammonia and then left
  8. customThe solution was thereafter evaporated
  9. customthe residue obtained
  10. customwas recrystallized from water