Ammonium formate → 8-ethoxy-3-ethyl-1-(3-hydroxypropyl)-1H-purine-2,6(3H,7H)-dione
Reaktionsgleichung
C([N:8]1[C:16]2[C:15](=[O:17])[N:14]([CH2:18][CH2:19][CH2:20][OH:21])[C:13](=[O:22])[N:12]([CH2:23][CH3:24])[C:11]=2[N:10]=[C:9]1[O:25][CH2:26][CH3:27])C1C=CC=CC=1.C([O-])=O.[NH4+]>C(O)C.[Pd]>[CH2:26]([O:25][C:9]1[NH:8][C:16]2[C:15](=[O:17])[N:14]([CH2:18][CH2:19][CH2:20][OH:21])[C:13](=[O:22])[N:12]([CH2:23][CH3:24])[C:11]=2[N:10]=1)[CH3:27]Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 80 °C
Versuchsvorschrift
7-benzyl-8-ethoxy-3-ethyl-1-(3-hydroxypropyl)-1H-purine-2,6(3H,7H)-dione (0.12 g, 0.323 mmol) was dissolved in ethanol (20 mL) and the mixture was degassed and refilled with nitrogen three times. Ammonium formate (0.5 g, 7.94 mmol) and 10% Pd/C (30 mg) were added. The mixture was again degassed and refilled with nitrogen three times; then it was warmed to 80° C. and stirred overnight. The mixture was cooled and filtered, and the filter cake was washed with methanol. The filtrate was concentrated to give 8-ethoxy-3-ethyl-1-(3-hydroxypropyl)-1H-purine-2,6(3H,7H)-dione (70 mg, 77.1% yield) as white solid. LCMS retention time 0.413 min; LCMS MH+ 283.
Aufarbeitung
- customthe mixture was degassed
- additionrefilled with nitrogen three times
- customThe mixture was again degassed
- additionrefilled with nitrogen three times
- temperatureThe mixture was cooled
- filtrationfiltered
- washthe filter cake was washed with methanol
- concentrationThe filtrate was concentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-4b3602e0cc5144ee83b0a9db2c6b83ef
- Quelldatensatz
- uspto-grants-2016_06
- Patentnummer
- US09359359B2
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