Reaktionsgleichung
Cl[C:2]1[N:3]=[C:4](Cl)[C:5]2[NH:10][N:9]=[C:8]([CH:11]([CH3:13])[CH3:12])[C:6]=2[N:7]=1.[OH:15][CH2:16][CH:17]([NH2:20])[CH2:18][CH3:19]>>[OH:15][CH2:16][CH:17]([NH:20][C:4]1[C:5]2[NH:10][N:9]=[C:8]([CH:11]([CH3:13])[CH3:12])[C:6]=2[N:7]=[C:2]([NH:20][CH:17]([CH2:16][OH:15])[CH2:18][CH3:19])[N:3]=1)[CH2:18][CH3:19]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 120 °C
Versuchsvorschrift
The mixture of 5,7-dichloro-3-isopropylpyrazolo[4,3-d]pyrimidine (100 mg; 0.331 mmol) and 2 mL 1-(R,S)-(hydroxymethyl)propylamine was heated at 120° C. for 6 hours. The reaction mixture was evaporated to dryness in vacuo. The product was purified by column chromatography on silica gel. The mixture of chloroform/methanol (96/4) was used as a mobile phase. Yield=80%; white syrupy; MS (ES+): 337.4 (100%, M+H+). 1H-NMR (300 MHz, CDCl3): 0.90-1.03 m (6H), 1.26 d (6H), 1.50-1.71 m (4H), 2.48 bs (1H), 3.07 m (1H), 3.40 m (1H), 3.59-3.90 m (4H).
Aufarbeitung
- customThe reaction mixture was evaporated to dryness in vacuo
- customThe product was purified by column chromatography on silica gel
- additionThe mixture of chloroform/methanol (96/4)
Quellen und Nachweise
- ORD-Eintrag
- ord-c82160b3f805470ab0df305563d1305c
- Quelldatensatz
- uspto-grants-2010_06
- Patentnummer
- US07745450B2
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