Реакция #1648

Уравнение реакции

sodium hydride

chloromethoxy(diethylphosphonomethoxy)methane

2-amino-6-chloropurine

→

title compound

2-Amino-6-chloro-9-[(diethylphosphonomethoxy)methoxymethyl]purine

Растворители

DMF

DMF

Условия реакции

Обработка

1. 1
   workup.STIRRINGAfter stirring 15 hr at 25° C.
2. 2
   Другоеvolatiles were removed in vacuo
3. 3
   Промывкаwashed with water (30 mL), brine
4. 4
   Сушкаdried (MgSO4)
5. 5
   ДругоеThe solvent was removed under reduced pressure
6. 6
   Другоеthe residual oil was chromatographed on silica gel

Методика

To a suspension of 60% sodium hydride in mineral oil (1.4 g, 34.5 mmol) in DMF (100 mL) was added 2-amino-6-chloropurine (5.78 g, 34.2 mmol) and the mixture was stirred for 1 hr at 25° C. To the resulting yellow solution was added dropwise a solution of above chloromethoxy(diethylphosphonomethoxy)methane in DMF (20 mL) under nitrogen. After stirring 15 hr at 25° C., volatiles were removed in vacuo. The residual oil was suspended in ethyl acetate (100 mL), washed with water (30 mL), brine and dried (MgSO4). The solvent was removed under reduced pressure, and the residual oil was chromatographed on silica gel using CH2Cl2 /3% MeOH as eluent to give the title compound as a colorless oil: yield 3.0 g (23%).

Источник