Reaktionsgleichung
[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4](Cl)[N:3]=1.[OH-].[Na+].[CH2:14]([OH:21])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>>[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([O:21][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:3]=1Komponenten
4
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
To a 500 mL 3 neck round bottom flask equipped with a magnetic stirrer, temperature probe and nitrogen inlet was added 2-amino-6-chloropurine (20 g), sodium hyroxide (28 g) and benzyl alcohol (200 mL). The mixture was stirred for 20 minutes and then heated at 100° C. for 2–3 hours. The reaction mixture was then cooled to room temperature and partitioned between methyl t-butyl ether (300 mL) and water (300 mL). The aqueous layer was separated and the pH was adjusted to 7–8 with 6 M HCl. The resulting solid was filtered, washed with water (50 mL) and dried under vacuum at 50° C. for 20 hours to provide the desired product as a pale yellow solid (24.3 g).
Aufarbeitung
- temperatureThe reaction mixture was then cooled to room temperature
- custompartitioned between methyl t-butyl ether (300 mL) and water (300 mL)
- customThe aqueous layer was separated
- filtrationThe resulting solid was filtered
- washwashed with water (50 mL)
- customdried under vacuum at 50° C. for 20 hours
Quellen und Nachweise
- ORD-Eintrag
- ord-00228ee92a4f40cf830b6553a46cef50
- Quelldatensatz
- uspto-grants-2007_03
- Patentnummer
- US07189849B2
Verknüpfte Notizen
Wird geladen…