Reaktion #220296

Reaktionsgleichung

Adenine

PMEA

adenine

ethylene carbonate

Magnesium Isopropoxide

→

9-(2-hydroxyethyl)adenine

Ausbeute 90.0%

Lösungsmittel

toluene

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction was cooled to below 50° C.
2. 2
   TemperaturThe slurry was further cooled to 5° C. for 2 hours
3. 3
   Filtrationfiltered
4. 4
   Waschenrinsed with toluene (2×)
5. 5
   SonstigeThe wet solid was dried in vacuo at 65° C.

Vorschrift

Adenine to PMEA using Magnesium Isopropoxide. To a suspension of adenine (16.8 g, 0.124 mol) in DMF (41.9 ml) was added ethylene carbonate (12.1 g, 0.137 mol) and sodium hydroxide (.100 g, 0.0025 mol). The mixture was heated at 130° C. overnight. The reaction was cooled to below 50° C. and toluene (62.1 ml) was added. The slurry was further cooled to 5° C. for 2 hours, filtered, and rinsed with toluene (2×). The wet solid was dried in vacuo at 65° C. to yield 20.0 g (90%) of 9-(2-hydroxyethyl)adenine as an off-white solid. Mp: 238-240° C.

Quelle