Reaktion #2117

Reaktionsgleichung

ammonia

trimethylsilyl bromide

[4-(7-ethoxymethyl-3-methylxanthin-1-yl)butyl]phosphonate

methanol

→

Diammonium [4-(7-ethoxymethyl-3-methylxanthin-1-yl)butyl]phosphonate

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe dichloromethane was then evaporated
2. 2
   Sonstigethe oily residue which remained was dried in a bulb tube in an oil pump vacuum
3. 3
   Sonstigeto remove excess trimethylsilyl bromide and ethyl bromide
4. 4
   Sonstigeformed
5. 5
   workup.STIRRINGstirred at room temperature for 2 hours
6. 6
   SonstigeAfter evaporating the solvent
7. 7
   Sonstigethe diammonium salt was crystallized from a methanoltdiisopropyl ether mixture

Vorschrift

3.4 ml (0.026 mol) of trimethylsilyl bromide were slowly added dropwise at 0° C., under an argon atmosphere, to a solution of 4.16 g (0.01 mol) of [4-(7-ethoxymethyl-3-methylxanthin-1-yl)butyl]phosphonate in 5 ml of dichloromethane. The solution was stirred at 0° C. for 1 hour and at room temperature for 2 hours. The dichloromethane was then evaporated and the oily residue which remained was dried in a bulb tube in an oil pump vacuum to remove excess trimethylsilyl bromide and ethyl bromide formed. The residue was taken up in a little methanol and treated with 1 ml of concentrated ammonia solution and stirred at room temperature for 2 hours. After evaporating the solvent, the diammonium salt was crystallized from a methanoltdiisopropyl ether mixture.

Quelle