Reaktionsgleichung
O.[NH2:2]N.Cl[C:5]1[N:13]=[CH:12][N:11]=[C:10]2[C:6]=1[NH:7][CH:8]=[N:9]2.[CH2:14]([N:16](C(C)C)[CH:17]([CH3:19])[CH3:18])C.[CH3:23][O:24]N(CCCNC1N=CN=C2C=1NC=N2)C>>[CH3:23][O:24][N:16]([CH:17]([CH3:19])[CH2:18][NH:2][C:5]1[N:13]=[CH:12][N:11]=[C:10]2[C:6]=1[NH:7][CH:8]=[N:9]2)[CH3:14]Komponenten
Versuchsvorschrift
In 15 ml of ethanol was dissolved 1.21 g (4.88 mmol) of the imide obtained in the above (1) and there was added 0.293 g (5.86 mmol) of hydrazine hydrate, followed by refluxing for 6 hours and cooling in an ice bath. The resulting solid was filtered off and the filtrate was concentrated to 2 ml by evaporator with a water bath at 5° C. This concentrated solution was mixed with 6 ml of n-butanol and to the mixture were added 0.528 g (3.42 mmol) of 6-chloropurine and 0.68 ml of ethyldiisopropylamine and the mixture was gently refluxed for 5 hours. This was cooled to room temperature and then the solvent was distiled off under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: chloroform/ethanol=9/1) to give 0.421 g (yield: 36%) of white crystals of N6 -[3-(N-methoxy-N-methylamino)propyl]adenine.
Aufarbeitung
- temperatureby refluxing for 6 hours
- temperaturecooling in an ice bath
- filtrationThe resulting solid was filtered off
- concentrationthe filtrate was concentrated to 2 ml by evaporator with a water bath at 5° C
- additionThis concentrated solution was mixed with 6 ml of n-butanol and to the mixture
- temperaturethe mixture was gently refluxed for 5 hours
- customthe solvent was distiled off under reduced pressure
- customThe residue was purified by column chromatography on silica gel (eluent: chloroform/ethanol=9/1)
Quellen und Nachweise
- ORD-Eintrag
- ord-478d26280dd042778a8b8e437feb89ca
- Quelldatensatz
- uspto-grants-1993_09
- Patentnummer
- US05244487
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