Reaktion #461088

Reaktionsgleichung

2,6-Diamino-9-[4-(diethoxyphosphoryl)butoxy]purine

bromotrimethylsilane

→

title compound

Ausbeute 84.0%

2,6-Diamino-9-(4-phosphonobutoxy)purine

Ausbeute 84.0%

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent was evaporated under vacuum
2. 2
   workup.DISSOLUTIONthe residue dissolved in methanol-water solution (8:2)
3. 3
   SonstigeThe material crystallised from the solution

Vorschrift

2,6-Diamino-9-[4-(diethoxyphosphoryl)butoxy]purine (0.07 g, 0.2 mmol) and bromotrimethylsilane (0.26 ml, 2 mmol) were dissolved in dimethylformamide (3 ml) and the reaction mixture was stirred at 23° C. for 4 hr. The solvent was evaporated under vacuum and the residue dissolved in methanol-water solution (8:2). The material crystallised from the solution to give the title compound as colourless crystals (0.05 g, 84%), m.p. 295°-297° C. 1H NMR: δH [(CD3)2SO+D2O] 1.68 (6H, m, CH2CH2CH2P), 4.31 (2H, t, J=6 Hz, NOCH2), 8.35 (1H, s, H-8).

Quelle